Purification process of N, O-1, 3-diacetyl indole

A technology of diacetyl indole and diacetyl indole, which is applied in the field of purification technology of N,O-1,3-diacetyl indole, can solve large waste solid pollution, nonconformity, column chromatography Difficulty in operation and other problems, to ensure product quality, avoid time-consuming, and avoid a lot of silica waste.

Active Publication Date: 2019-06-28
CHANGZHOU VOCATIONAL INST OF ENG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] 1) The purity of the obtained product is about 80%, and the distribution coefficient difference between the product, by-products and raw materials in water or common organic solvents is relatively small. Using common crystallization method, the purity is not more than 90%. Crystallization efficiency is low and time-consuming
[0004] 2) Another method for purifying N,O-1,3-diacetylindole is to use silica gel for column chromatography. If a large amount of purification is performed, the amount of silica gel used will be large and will cause large waste solid pollution. It does not meet the requirements of the current green chemical industry; using a large amount of solvents at the same time will cause a large amount of waste liquid discharge or high waste liquid treatment costs; the operation of column chromatography is difficult, and senior operators are required, and the personnel cost is high

Method used

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  • Purification process of N, O-1, 3-diacetyl indole

Examples

Experimental program
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Effect test

Embodiment 1

[0026] The crude product of N,O-1,3-diacetylindole with a purity of 80% is used as a raw material, and the purification process of a kind of N,O-1,3-diacetylindole of the present invention is adopted for purification, which comprises the following steps: Follow the steps below:

[0027]S1: Pretreatment, place the three-necked flask in an ultrasonic constant temperature water bath, start the stirrer, add 400 g of dichloromethane into the three-necked flask, and control the temperature of dichloromethane to be 30±2°C, add 60 g of N to the three-necked flask , The crude product of O-1,3-diacetyl indole was stirred for 30min, the three-necked flask was placed in a refrigerator of -18°C for 30min, and filtered to obtain the crude product of N,O-1,3-diacetyl indole 43g and primary filtrate;

[0028] S2: configure a slurry, mix dichloromethane and anhydrous methanol according to a volume ratio of 7:1, stir evenly to obtain a slurry, and the polarity of the slurry is 6 to 6.2;

[00...

Embodiment 2

[0033] The difference between Example 2 and Example 1 is that in the step S1, the N,O-1,3-diacetyl indole crude product input amount is 1kg, and the methylene chloride addition is 6kg to obtain N,O-1 , 720g of 3-diacetyl indole primary product; in the step S2, the added amount of the slurry is 2.2kg; in the step S4, the low-temperature drying temperature is 5°C, to obtain a white N,O-1 with a purity of 98.5%, The finished product of 3-diacetyl indole is 700g, and the total time is 5h.

Embodiment 3

[0035] The difference between Example 3 and Example 1 is that in the step S1, the N,O-1,3-diacetyl indole crude product input amount is 2kg, and the methylene chloride addition is 10kg to obtain N,O-1 , 1.5kg of the first product of 3-diacetyl indole; in the step S2, the added amount of the slurry is 4.5kg; in the step S4, the low-temperature drying temperature is 0° C. to obtain a white N,O-1 with a purity of 98%. ,3-Diacetyl indole finished product is 1.41kg, and the total time is 8h.

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Abstract

The invention discloses a purification process of N, O-1, 3-diacetyl indole. The process comprises four procedures of pretreatment, pulping liquid preparation, pulping, impurity removal and post-treatment. The process is simple in operation steps and high in practicability; in particular, a mixed liquid pulping method is adopted to replace a traditional recrystallization method, so that the purification efficiency of the N, O-1, 3-diacetyl indole is improved, the defects of long time consumption and multiple types of solvents of the traditional repeated recrystallization are overcome, at the same time, the generation of a large amount of silica gel waste residues when silica gel column chromatography is used for purification is avoided, and the requirements of environment-friendly chemistry are met; and the solvent polarity of the pulping liquid used in the process is 6-6.2, so that the N, O-1, 3-diacetyl indole is simply separated from other substances so as to obtain a product with higher purity, and the product quality is guaranteed.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a purification process of N,O-1,3-diacetyl indole. Background technique [0002] N,O-1,3-Diacetylindole is a kind of API, and it can also be used as a pharmaceutical intermediate to synthesize other drugs. At present, the commonly used synthesis method of N,O-1,3-diacetyl indole is to carry out substitution reaction of o-chlorobenzoic acid and glycine, and then carry out neutralization reaction with acetic anhydride, and finally undergo a ring-forming reaction in acetic anhydride to form be made of. However, this synthesis method currently has the following problems: [0003] 1) The purity of the obtained product is about 80%, and the distribution coefficient gap between the product, by-product and the raw material in water or common organic solvent is small, using the common crystallization method, the purity is not more than 90%, using a variety of solvents to repe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D209/36
Inventor 蒋若愚龚玲刘长春程进
Owner CHANGZHOU VOCATIONAL INST OF ENG
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