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Preparation method for N-benzyloxycarbonyl-2-amino-1-propanol

A benzyloxycarbonyl and amino group technology, applied in the field of compound preparation, can solve the problems of unsuitability for industrial production, low synthesis yield, large pollution, etc., and achieve the effects of precise control of reaction temperature, rapid reaction, and strong mass transfer ability

Inactive Publication Date: 2019-09-13
南京博源医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] N-benzyloxycarbonyl-2-amino-1-propanol is an important drug synthesis intermediate. In the development of drugs, conventional reactors are used to produce N-benzyloxycarbonyl-2-amino-1-propanol , there are disadvantages such as low synthesis yield and large pollution, so it is not suitable for industrial production

Method used

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Examples

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Effect test

preparation example Construction

[0027] A preparation method of N-benzyloxycarbonyl-2-amino-1-propanol, comprising the following steps:

[0028] (1) Add ammonia water to the reactor, add catalyst and propylene oxide after cooling down, heat up and pressurize, and heat to reflux to obtain 1-amino-2-propanol;

[0029] (2) Add 1-amino-2-propanol and benzyl chloroformate into a mixer filled with solvent to form a mixed solution. After the mixed solution material is reacted in a microchannel reactor, the material is discharged and the reaction is terminated. After the low boilers are removed by the degassing tower, N-benzyloxycarbonyl-2-amino-1-propanol is obtained.

Embodiment 1

[0031] A preparation method of N-benzyloxycarbonyl-2-amino-1-propanol, comprising the following steps:

[0032] (1) Add 500mL of ammonia water into the reactor, cool down to 0°C, add 2g of formic acid and 50g of propylene oxide, heat up to 50°C, pressurize to 1MPa, react for 4h to obtain 1-amino-2-propanol;

[0033] (2) Add 6.10g of 1-amino-2-propanol and 17.5g of benzyl chloroformate into a mixer containing 200mL of dichloromethane to form a mixed liquid, and pass the mixed liquid material through the pre-reaction of the microchannel reactor After filtering, it enters the reaction section of the microchannel reactor. The temperature in the reaction section is 10°C, the pressure is 1MPa, and the material residence time is 1s. After the reaction, the material is discharged, the reaction is terminated, and the low-boiling After the product, N-benzyloxycarbonyl-2-amino-1-propanol was obtained.

Embodiment 2

[0035] A preparation method of N-benzyloxycarbonyl-2-amino-1-propanol, comprising the following steps:

[0036] (1) Add 500mL of ammonia water into the reactor, cool down to 0°C, add 2g of formic acid and 50g of propylene oxide, heat up to 100°C, pressurize to 1MPa, and react for 3h to obtain 1-amino-2-propanol;

[0037] (2) Add 6.10g of 1-amino-2-propanol and 26.25g of benzyl chloroformate into a mixer containing 200mL of dichloromethane to form a mixed liquid, and pass the mixed liquid material through the pre-reaction of the microchannel reactor After filtering, it enters the reaction section of the microchannel reactor. The temperature in the reaction section is 30°C, the pressure is 0.5MPa, and the material residence time is 0.5s. After the reaction, the material is discharged, the reaction is terminated, and the degassing tower After low boilers, N-benzyloxycarbonyl-2-amino-1-propanol is obtained.

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Abstract

The invention discloses a preparation method for N-benzyloxycarbonyl-2-amino-1-propanol. The preparation method comprises the following steps: adding ammonia water into a reactor, adding a catalyst and epoxypropane after cooling, carrying out heating and pressurization, and performing heating reflux to obtain 1-amino-2-propanol; and adding 1-amino-2-propanol and benzyl chloroformate into a solvent-containing mixer to prepare a mixed solution, allowing the mixed solution to undergo a reaction via a microchannel reactor, then carrying out discharging, terminating the reaction and removing low-boiling-point substances via a degassing column so as to obtain N-benzyloxycarbonyl-2-amino-1-propanol. The preparation method of the invention realizes high preparation yield of N-benzyloxycarbonyl-2-amino-1-propanol through two-step operation and is simple in preparation process; and through fast reaction in the microchannel reactor, reaction time is greatly reduced, reaction efficiency is improved, and the conversion rate of raw materials and product yield are enhanced.

Description

technical field [0001] The invention relates to N-benzyloxycarbonyl-2-amino-1-propanol, belonging to the technical field of compound preparation. Background technique [0002] 1-Amino-2-propanol is an important chemical intermediate, which is widely used in water treatment, medicine, pesticide, etc. Patent CN105289027A discloses a continuous method, which uses high ammonia ring ratio and high temperature reaction conditions to prepare 1-amino-2-propanol, and reacts the reaction materials with high ammonia ring ratio reflux. In this method, the molar ratio of ammonia to propylene oxide is 30-300:1. Too high a ring ratio of ammonia prevents a large amount of ammonia from fully reacting, resulting in many by-products, and the cost of treating the reaction tail gas is relatively high. [0003] Microchannel reactors have excellent heat and mass transfer capabilities, and can achieve instant uniform mixing of materials and efficient heat transfer, so many reactions that cannot be...

Claims

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Application Information

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IPC IPC(8): C07C213/04C07C215/08C07C269/04C07C271/16B01J19/00
CPCC07C213/04C07C269/04B01J19/0093C07C215/08C07C271/16
Inventor 陈建国张国品
Owner 南京博源医药科技有限公司
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