- Synthesis method of diethyl cyanomethylphosphonate
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The invention discloses a synthesis method of diethyl cyanomethylphosphonate. The synthesis method comprises the following steps: carrying out an esterification reaction on chloroacetic acid and ethanol to obtain ethyl chloroacetate; reacting the ethyl chloroacetate with ammonia water to generate chloroacetamide; adding phosphorus pentoxide into the chloroacetamide, performing heating dehydration,distilling out chloroacetonitrile while heating, and finally performing reduced pressure distillation to enable the chloroacetonitrile to be completely distilled out; transferring the chloroacetonitrile into a synthesis reaction kettle, adding a catalyst tetrabutylammonium iodide, heating, dropwise adding triethyl phosphite, and controlling the internal temperature for a reaction to obtain a crude product; and transferring the crude product into a high-purity rectifying tower, and performing purification to respectively rectify triethyl phosphite and diethyl cyanomethylphosphonate.
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Paragraph 0016; 0018-0020; 0022-0024; 0026-0028; 0030-0031
(2020/05/01)
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- (S)-1-Boc-3-hydroxypiperidine synthesis method
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The invention discloses a (S)-1-Boc-3-hydroxypiperidine synthesis method. The method utilizes (R)-glyceraldehyde acetonide as a raw material. Through witting reaction-based acetonitrile group addition, palladium-carbon-based double bond reduction, deprotection, p-tosyl selective addition, Raney nickel-based hydrogenation reduction of the nitrile group along with ring closing, and piperidine ring nitrogen Boc protection, the (S)-1-Boc-3-hydroxypiperidine is obtained. The method utilizes the cheap chiral raw material as a starting material, produces a chiral product and prevents large material consumption and a yield loss of a splitting technology.
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Paragraph 0049
(2016/12/01)
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