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Continuous synthesis method of ethyl 3-oxo-3-hydrazino-propionate

A technology of ethyl hydrazinopropionate and its synthesis method, which is applied in the field of continuous synthesis of ethyl 3-oxo-3-hydrazinopropionate, and can solve problems such as high energy, large amount of hydrazine hydrate, and poor selectivity

Pending Publication Date: 2021-09-14
SUZHOU INDAL PARK INST OF SERVICES OUTSOURCING
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] For the problems referred to above, the purpose of the present invention is to provide the continuous synthesis method of ethyl 3-oxo-3-hydrazine propionate, which solves the long reaction time of traditional kettle, poor selectivity and low yield, and also solves the problem of hydrazine hydrate in The safety problem of large quantity and large energy in the reaction process realizes green and safe chemistry

Method used

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  • Continuous synthesis method of ethyl 3-oxo-3-hydrazino-propionate
  • Continuous synthesis method of ethyl 3-oxo-3-hydrazino-propionate
  • Continuous synthesis method of ethyl 3-oxo-3-hydrazino-propionate

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Embodiment 1

[0040] Such as figure 1 As shown, ethanol and diethyl malonate are pumped to temperature zone 1 (10°C) respectively to form an ethanol solution of raw materials; the flow rate of ethanol is 4mL / min, and the flow rate of diethyl malonate is 1mL / min. Hydrazine hydrate (50wt%) was pumped to temperature zone 2 for pre-cooling to 10°C, with a flow rate of 0.5mL / min. Afterwards, the hydrazine hydrate solution and the ethanol solution of the raw materials are transported into the tubular reactor for hydrazination reaction (temperature zone 3, 10° C.), and the reaction residence time is 50 minutes. The reaction solution flows out into the Raney nickel fixed bed for quenching (temperature zone 4, 60° C.), and the quenching residence time is 15 minutes. After the system reached steady state, samples were collected for 60 minutes. The effluent solution was concentrated, crystallized, and vacuum-dried at 40° C. to obtain 12.50 g of product with a purity of 99.0% and a yield of 21.5%.

Embodiment 2

[0042] Such as figure 2 As shown, methanol and diethyl malonate are pumped to temperature zone 1 (20°C) respectively to form a methanol solution of raw materials; the flow rate of methanol is 50mL / min, and the flow rate of diethyl malonate is 50mL / min. Hydrazine hydrate (80wt%) was pumped to temperature zone 2 for pre-cooling to 20°C, with a flow rate of 12mL / min. Afterwards, the hydrazine hydrate solution and the methanol solution of the raw materials are transported into the microchannel reactor for hydrazination reaction (temperature zone 3, 20° C.), and the reaction residence time is 30 minutes. The reaction solution flows out into the Raney nickel fixed bed for quenching (temperature zone 4, 80° C.), and the quenching residence time is 12 minutes. After the system reached steady state, samples were collected for 60 minutes. The effluent solution was concentrated, crystallized, and vacuum-dried at 40°C to obtain 549.5 g of the product with a purity of 98.8% and a yield ...

Embodiment 3

[0044] Such as image 3As shown, diethyl malonate is pumped to temperature zone 1 (110°C), and the flow rate of diethyl malonate is 50mL / min. Hydrazine hydrate (80wt%) was pumped to temperature zone 2 to preheat to 110°C, and its flow rate was 0.8mL / min. Afterwards, the hydrazine hydrate solution and the raw material solution are transported into the microchannel reactor for hydrazination reaction (temperature zone 3, 130° C.), the reaction residence time is 10 s, and the pressure is 12 kG. The reaction solution flows out into the Raney nickel fixed bed for quenching (temperature zone 4, 150°C), and the quenching residence time is 7s; the reaction solution enters the short-path still for separation, and the unreacted diethyl malonate is obtained by the short-path still. Enter Repeat Application. After the system reached steady state, samples were collected for 24 hours. The effluent solution was concentrated, crystallized, and vacuum-dried at 40° C. to obtain 760 g of a pro...

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Abstract

The invention discloses a continuous synthesis method of ethyl 3-oxo-3-hydrazino-propionate, which comprises the steps of taking diethyl malonate and a hydrazine reagent as raw materials, and carrying out preheating, hydrazine reaction and quenching to obtain ethyl 3-oxo-3-hydrazino-propionate. The continuous synthesis method is carried out in a continuous reactor. The method provided by the invention solves the problems of long reaction time, poor selectivity and low yield of a traditional kettle, also solves the safety problems of large quantity and large energy of hydrazine hydrate in the reaction process, and realizes green and safe chemistry.

Description

technical field [0001] The invention belongs to the technical field of organic chemistry and relates to a preparation process of a pharmaceutical intermediate, in particular to a continuous synthesis method of ethyl 3-oxo-3-hydrazinopropionate. Background technique [0002] Ethyl 3-oxo-3-hydrazinopropionate is a commonly used chemical intermediate in the field of organic synthesis. It is mainly used in the oxadiazole skeleton in agrochemical or biomedicine. The ester structure is as follows: [0003] [0004] The synthesis of ethyl 3-oxo-3-hydrazinopropionate usually uses diethyl malonate as a raw material through direct hydrazination of hydrazine hydrate. [0005] [0006] Yet adopt batch or semi-batch process to produce ethyl 3-oxo-3-hydrazinopropionate, there are following problems usually: [0007] a) The efficiency of batch batch operation is not high, the reaction time is very long, the reaction selectivity is poor, and there are many by-products. [0008] b) ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C241/04C07C243/28
CPCC07C241/04C07C243/28
Inventor 关炜佳
Owner SUZHOU INDAL PARK INST OF SERVICES OUTSOURCING
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