1. 2 Steps
Overview
Steps/Stages Notes
1.1C:Hexamethylentetramine, S:H2O, rt → 260°C; 260°C, 100 bar;
260°C, 100 bar → 250 bar; 1 h, 260°C, 250 bar; 260°C → rt
2.1R:H2, C:Pd, C:Se, 10-100 min, 80°C
1) autoclave ud, 2) flow system, Reactants:
2, Reagents: 1, Catalysts: 3, Solvents: 1,
Steps: 2, Stages: 2, Most stages in any one
step: 1
References
Continuous method for producing citral
By Wegner, Guenter et al
From PCT Int. Appl., 2008037693, 03 Apr
2008
开胃菜花
Experimental Procedure
Step 1
Example 1: Preparation of 3-methyl-3-buten-1-ol (MBE) in 3000 ml autoclave. Starting products: 2053
g (36.7 mol) of isobutene (from a steel flask), 200 g (3, 3 mol) of formaldehyde (aqueous solution,
50%), 1.4 g urotropin solution (aqueous 15%). 1a) Procedure of the reaction: The formaldehyde
solution and isobutene from a steel flask were filled into an autoclave and the autoclave was clod.
The autoclave was heated to 260°C, where a internal pressure was created by about 100 bar. Then
the autoclave was presd with nitrogen to about 250 bar. The mixture was stirred at about 260°C and
about 250 bar for one hour. After an hour, the mixture was cooled down to room temperature and
depressurized. Relead substance isobutene was absorbed (about 1800 g) and could be ud for
other mixtures. The liquid reaction discharge was weighed and analyzed. A discharge was produced
from: the upper pha: 370 g and lower pha: 29 g, in which an analytical asssment was resulted
as following: upper pha: 270.1 g (73%) of MBE, 3.7 g (1%) of formaldehyde, 74.0 g (20%) of water,
手机翻新机22.2 g (6%) of by-products. lower pha: 2.3 g (8%) of MBE, 26.7 g (92%) of water. Conversion of
formaldehyde: 96.3%; lectivity to MBE: 98.6%. 1b) pure distillation of MBE: The distillation was
carried out in a 2 liter double jacketed four-necked flask equipped with a thermostat, column (with 1 m
of Sulzer EX-packing), reflux splitter, vacuum pumps, distillation receivers, thermometer and cold trap
with dry ice. Starting product: 1110 g of discharged upper pha from the Autoclave experiment 1a)
taken into the bottom flask (for the distillation cartridge 1b) were ud 3 autoclave discharge 1a.
Procedure: The water paration was taken place under normal pressure (1013 mbar) at a bottom
temperature to 135°C and a transition temperature up to 101°C. The reflux ratio in this ca was about
5:1. Fraction 1:430 g (2-pha); analysis: 215 g (50%) of water, 193.5 g (45%) of MBE. The
purification of MBE was carried out then by distillation at a pressure of about 100 mbar at a bottom
temperature of about 155°C and a transition temperature up to about 73°C. The reflux ratio in this ca
was about 5:1. Here two fractions were obtained: fraction 2:50 g; Analysis: 25g (50%) of formaldehyde,
25 g (50%) of MBE. The yield of bottom discharge after the distillation end was 40 g. The fraction 1
and 2 could be possibly ud for further distillation.
Step 2
Example 4: Preparation of 3-methyl-2-buten-ol (prenol) from MBE by catalytic isomerization. 4a)
Isomerization reaction: For the isomerization of MBE to give prenol on a Pd/Se catalyst, a tubular
reactor is ud. Starting material: 1000 g MBE. 60 ml of catalyst (Pd/Se on a ceramic carrier) is filled
into the tubular reactor. The apparatus is inerted with nitrogen. The tubular reactor is heated to about
80 °C. Then, about 100g/h of MBE and about 5 l/h of hydrogen are pasd from the bottom through
the reactor. After a reaction time of 10 to 100 minutes, reveals the following: Conversion: about 55%,
lectivity: about 91%. The discharge is: 1000 g; analysis: 470.0 g (47%) MBE, 500.0 g (50%) prenol,
25.0 g (2.5%), iso-amyl alcohol. 4 b) Purification of prenol by distillation: Starting material: 1000 g of
isomerization discharge from Example 4a). In a 2 liter double jacket four-necked flask equipped with
thermostat, 1 m column (with Sulzer EX-packing), reflux divider, vacuum pumps, distillation receivers,
thermometer and cooling trap, The purification by distillation is carried out at a vacuum of about 500
mbar. In this process, the low boiling contents and the unreacted MBE are distilled off upto a overhead
temperature of about 107°C. The reflux ratio in this ca is approximately 10:1. Fraction 1 (low boiling
components and MBE): 501 g; analysis: 35.1 g (7%) low boiling components, of which about 25 g of
iso-amyl alcohol, 460.9 g (92%) of MBE. 5.0 g (1%) prenol. The thus recycled MBE is ud together
with the low boiling components (especially isoamyl alcohol) preferably in the synthesis of MBA. The
purification of prenol by distillation is carried out at a bottom temperature upto 165°C, a vacuum of 500
mbar and an overhead temperature to 122°C. The reflux ratio here is 5:1. Fraction 2 (prenol): 470 g;
analysis: 2.4 g (0.5%) MBE, 467.7 g (99.5%) prenol. The bottom product is 9 g.
CASREACT ®: Copyright © 2015 American Chemical Society. All Rights Rerved. CASREACT contains reactions from CAS and from: ZIC/VINITI databa (1974-1999) provided by InfoChem; INPI data prior to 1986; Biotransformations databa compiled under the direction of Professor Dr. Klaus Kieslich; organic reactions, portions copyright 1996-2006 John Wiley & Sons, Ltd., John Wiley and Sons, Inc., Organic Reactions Inc., and Organic Synthes Inc. Reproduced under licen. All Rights Rerved.
2. 2 Steps
Overview
Steps/Stages Notes
1.1R:Hexamethylentetramine, S:H2O, 1 h, 260°C, 250 bar
2.1R:H2, C:Pd, C:Se, 100 min, 80°C
1) alternative reaction conditions shown,
autoclave ud, high pressure, 2) catalyst on
ceramic support, Reactants: 2, Reagents: 2,
Catalysts: 2, Solvents: 1, Steps: 2, Stages: 2,
Most stages in any one step: 1
References
Continuous method for preparation of citral
油菜菌核病By Anon.
Journal, 6(11A), 9; 2006 CASREACT ®: Copyright © 2015 American Chemical Society. All Rights Rerved. CASREACT contains reactions from CAS and from: ZIC/VINITI databa (1974-1999) provided by InfoChem; INPI data prior to 1986; Biotransformations databa compiled under the direction of Professor Dr. Klaus Kieslich; organic reactions, portions copyright 1996-2006 John Wiley & Sons, Ltd., John Wiley and Sons, Inc., Organic Reactions Inc., and Organic Synthes Inc. Reproduced under licen. All Rights Rerved.
3. Single Step
Overview
Steps/Stages Notes
1.1C:Bu2Sn dilaurate
1.2C:947-19-3, C:7473-98-5
e details, product depends on reactants,
photochemical (UV, stage 2), Reactants: 5,
Catalysts: 3, Steps: 1, Stages: 2, Most stages
in any one step: 2
References
Two-step curable polymer compositions for
optical materials and their cured products
By Nakamura, Satoshi and Morozumi,
Yasutaka
From Jpn. Kokai Tokkyo Koho, 2012077278,
19 Apr 2012
CASREACT ®: Copyright © 2015 American Chemical Society. All Rights Rerved. CASREACT co
ntains reactions from CAS and from: ZIC/VINITI databa (1974-1999) provided by InfoChem; INPI data prior to 1986; Biotransformations databa compiled under the direction of Professor Dr. Klaus Kieslich; organic reactions, portions copyright 1996-2006 John Wiley & Sons, Ltd., John Wiley and Sons, Inc., Organic Reactions Inc., and Organic Synthes Inc. Reproduced under licen. All Rights Rerved.
4. Single Step
Overview
Steps/Stages Notes
理想流沙河1.1C:Bu2Sn dilaurate
1.2C:947-19-3, C:7473-98-5
e details, product depends on reactants,
photochemical (UV, stage 2), Reactants: 5,
Catalysts: 3, Steps: 1, Stages: 2, Most stages
in any one step: 2
References
Two-step curable polymer compositions for
optical materials and their cured products
By Nakamura, Satoshi and Morozumi,
Yasutaka
From Jpn. Kokai Tokkyo Koho, 2012077278,
19 Apr 2012
CASREACT ®: Copyright © 2015 American Chemical Society. All Rights Rerved. CASREACT contains reactions from CAS and from: ZIC/VINITI databa (1974-1999) provided by InfoChem; INPI data prior to 1986; Biotransformations databa compiled under the direction of Professor Dr. Klaus Kieslich; organic reactions, portions copyright 1996-2006 John Wiley & Sons, Ltd., John Wiley and Sons, Inc., Organic Reactions Inc., and Organic Synthes Inc. Reproduced under licen. All Rights Rerved.
5. Single Step
Overview
Steps/Stages Notes
1.1R:Cyanuric acid, R:SiO2, C:931-36-2, 60 min, rt; 180 min, 60°C
Reactants: 2, Reagents: 2, Catalysts: 1, Steps:
1, Stages: 1, Most stages in any one step: 1
References
Curable adhesives with good recyclability and
reworkability and method for disasmbling
structures bonded with them by hand
By Namba, Chie et al
From PCT Int. Appl., 2013047046, 04 Apr
2013
CASREACT ®: Copyright © 2015 American Chemical Society. All Rights Rerved. CASREACT contains reactions from CAS and from: ZIC/VINITI databa (1974-1999) provided by InfoChem; INPI data prior to 1986; Biotransformations databa compiled under the direction of Professor Dr. Klaus Kieslich; organic reactions, portions copyright 1996-2006 John Wiley & Sons, Ltd., John Wiley and Sons, Inc., Organic Reactions Inc., and Organic Synthes Inc. Reproduced under licen. All Rights Rerved.
6. Single Step
Overview
花开时节又逢君>方便抽样Steps/Stages Notes
1.1 R:
rt → 120°C
1.2 2 min, 120°C
1.3 2 min, 120°C
Reactants: 3, Reagents: 1, Steps: 1, Stages:
3, Most stages in any one step: 3
References
Compatibilized blends of a thermoplastic方文杰
elastomer and a polyolefin
By Farkas, Julius et al
From PCT Int. Appl., 9919406, 22 Apr 1999
CASREACT ®: Copyright © 2015 American Chemical Society. All Rights Rerved. CASREACT contains reactions from CAS and from: ZIC/VINITI databa (1974-1999) provided by InfoChem; INPI data prior to 1986; Biotransformations databa compiled under the direction of Professor Dr. Klaus Kieslich; organic reactions, portions copyright 1996-2006 John Wiley & Sons, Ltd., John Wiley and Sons, Inc., Organic Reactions Inc., and Organic Synthes Inc. Reproduced under licen. All Rights Rerved.
7. Single Step
>航母造价多少亿
