A kind of method for continuous and rapid synthesis of 5-(β-methylthioethyl)-hydantoin

A technology of methylthioethyl and hydantoin, applied in organic chemistry, products, reagents, etc., can solve the problems of lack of economical efficiency, easy polymerization of raw material cyanohydrin, easy generation of by-products, etc. The effect of depolymerization and its by-product formation, shortening reaction time, and increasing intermolecular collisions

Active Publication Date: 2022-08-09
LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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Problems solved by technology

[0006] In view of the above-mentioned shortcoming of the prior art, the object of the present invention is to provide a kind of method for synthesizing 5-(β-methylthioethyl)-hydantoin, this method possesses atom economy, is used to solve the present problem In the prior art, when synthesizing 5-(β-methylthioethyl)-hydantoin, the reaction time is long, a large amount of ammonium bicarbonate is excessive, the raw material cyanohydrin is easy to polymerize and by-products are easily produced, and the reaction rate is slow, resulting in the formation of colored impurities , Insufficient response, not economical and economical, resulting in waste of resources, not green and environmental protection, etc.

Method used

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  • A kind of method for continuous and rapid synthesis of 5-(β-methylthioethyl)-hydantoin
  • A kind of method for continuous and rapid synthesis of 5-(β-methylthioethyl)-hydantoin
  • A kind of method for continuous and rapid synthesis of 5-(β-methylthioethyl)-hydantoin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 Two-component reaction of cyanohydrin-ammonium bicarbonate aqueous solution

[0028] 93.711 g (0.5 mol) of 2-hydroxy-4-methylthiobutyronitrile aqueous solution (cyanohydrin) with a mass percentage content of 70 wt % and ammonium bicarbonate aqueous solution with ammonia and carbon dioxide contents of 7.5 wt % and 18.53 wt % respectively 124.667 g (cyanohydrin:ammonia:carbon dioxide=1.0:1.10:1.05) was pumped into the microchannel reactor loaded with catalyst N10 through a metering pump at the same time, the flow rate of cyanohydrin in the microchannel was 2.5ml / min, and the ammonium bicarbonate aqueous solution was The flow rate in the microchannel is 3.33ml / min, the temperature of the control reaction is 80°C, the pressure is 0.55MPa, the residence time is 3min (that is, the time for the reaction liquid to flow through the microchannel), and the outflow liquid is clear, colorless and transparent 5 -(β-Methylthioethyl)-hydantoin aqueous solution (hydantoin) 218...

Embodiment 2

[0046] Example 2 Three-component reaction of methylthiopropionaldehyde, sodium cyanide, and ammonium bicarbonate aqueous solution

[0047] 52.3473 g (0.5 mol) of methylthiopropionaldehyde with a mass percentage of 99.5 wt %, 82.4833 g (0.505 mol) of an aqueous sodium cyanide solution with a mass percentage of 30 wt %, and ammonia and carbon dioxide with a content of 7.5 wt % respectively. and 124.667 g of 18.53 wt% ammonium bicarbonate aqueous solution (methylthiopropionaldehyde: sodium cyanide: ammonia: carbon dioxide = 1.0: 1.01: 1.10: 1.05) simultaneously through a metering pump into the microchannel reactor loaded with catalyst N10, The flow rate of methylthiopropionaldehyde in the microchannel is 2.5ml / min, the flow rate of the aqueous sodium cyanide solution in the microchannel is 3.9393ml / min, and the flow rate of the aqueous ammonium bicarbonate solution in the microchannel is 5.954ml / min, controlling the reaction The temperature is 100°C, the pressure is 1.10MPa, the ...

Embodiment 3

[0048] Example 3 Three-component reaction of methylthiopropionaldehyde, potassium cyanide and ammonium bicarbonate aqueous solution

[0049] 52.3473 g (0.5 mol) of methylthiopropionaldehyde with a mass percentage of 99.5 wt %, 93.9531 g (0.505 mol) of an aqueous potassium cyanide solution with a mass percentage of 35 wt %, and ammonia and carbon dioxide with a content of 7.5 wt % respectively. and 124.667 g of 18.53 wt% ammonium bicarbonate aqueous solution (methylthiopropionaldehyde: potassium cyanide: ammonia: carbon dioxide = 1.0: 1.01: 1.10: 1.05) simultaneously through a metering pump into the microchannel reactor loaded with catalyst N10, The flow rate of methylthiopropionaldehyde in the microchannel is 2.5ml / min, the flow rate of the potassium cyanide aqueous solution in the microchannel is 4.487ml / min, and the flow rate of the aqueous ammonium bicarbonate solution in the microchannel is 5.954ml / min, controlling the reaction The temperature is 90°C, the pressure is 1.0M...

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Abstract

The present invention provides a method of synthetic 5 一 (β‑ methamphetamine) ‑ ‑ 乙 乙 本 本, including: 2‑ hydroxyl ‑ 4‑ methyl sulfinin (or 3‑ gonosulfonal propane, cyanide, cyanide cyanide, cyanide,Chemicals) react with the micro -channel reactor of the load catalyst with the measuring pump of the ammonium carbide water solution. The control reaction temperature is 60 ° C to 120 ° C, the pressure is 0.5MPa ~ 1.0MPa, and the residence time of the reactor in the micro -channel is 1~ 10min, directly obtain 5‑ (β -methyl sulfur ethyl) in the post -application process.The present invention prepares 5‑ (β‑ methylvyl ethyl) in a micro -channel reactor of a load catalyst to reduce the use of 30 ~ 50%ammonium carbonate solution.To remove ammonia, the atomic utilization rate is high, and efficiently clean; does not require the heating at the stage, which greatly shortens the circular reaction time, reduces the heating polymerization polymerization of 2‑ hydroxyl ‑ 4‑ 4‑ 4‑.The rate is increased to more than 99%.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a method for synthesizing 5-(β-methylthioethyl)-hydantoin. technical background [0002] 5-(β-Methylthioethyl)-hydantoin, or hydantoin for short, is an important intermediate in the chemical synthesis of DL-methionine. At present, there are two main methods for preparing 5-(β-methylthioethyl)-hydantoin: the first is the "three-component" reaction synthesis method, that is, the alkali metal hydrocyanic acid or hydrocyanic acid is used. The molar ratio of salt to methylthiopropionaldehyde and ammonium bicarbonate is: hydrocyanic acid: methylthiopropionaldehyde: ammonia: carbon dioxide=1.0~1.1:1.0:2.0~2.6:1.5~2.0, a large amount of ammonium bicarbonate is excessive, After three stages of heating, 58°C, 90°C and 138°C respectively, the reaction pressure is 0.8MPa-2.0MPa, and the total reaction time is 15-30min, after stripping the excess ammonia and carbon dioxide that did not parti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D233/76
CPCY02P20/584
Inventor 周荣超廖常福彭启明周荣敏
Owner LUFENG TIANBAO PHOSPHORUS CHEM CO LTD
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