Acetic Acid → Ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinate

HRID 5165

반응식

HRID 5165 반응식
[CH2:1]([O:3][CH:4]([P:8]([O-:12])[O:9][CH2:10][CH3:11])[O:5][CH2:6][CH3:7])[CH3:2].[C:13](#[N:17])/[CH:14]=[CH:15]/[CH3:16].[H-].[Na+].C(O)(=O)C>C(O)C>[C:13]([CH2:14][CH:15]([P:8]([CH:4]([O:5][CH2:6][CH3:7])[O:3][CH2:1][CH3:2])(=[O:12])[O:9][CH2:10][CH3:11])[CH3:16])#[N:17]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 24758Sodium hydrideHCID 637921CrotononitrileHCID 85631043Ethyl(diethoxymethyl)phophonite

생성물 1

HCID 14362805Ethyl 1-methyl-2-cyanoethyl(diethoxymethyl)phosphinate

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

A solution of 23.5 g of ethyl (diethoxymethyl)phosphonite and 6.7 g of crotononitrile in 30 ml of dry ethanol is added to a stirred mixture of 1.2 g of sodium hydride (50% dispersion in oil) in 30 ml of ethanol at 0° C. under an atmosphere of nitrogen. The reaction mixture is allowed to warm to room temperature and stirred for 4 hours. 1 ml of glacial acetic acid is added and the mixture concentrated under reduced pressure. The resulting crude product is dissolved in 50 ml of ethyl acetate, washed twice with 25 ml of water, and the organic extract is dried over magnesium sulphate, and then concentrated under reduced pressure. The crude product is distilled under reduced pressure to give ethyl 2-cyano-1methylethyl(diethoxymethyl)phosphinate, b.p. 116° C./0.01 mbar, 31P=+42.2 and +42.0 ppm (CDCl3).

후처리

  1. concentrationthe mixture concentrated under reduced pressure
  2. dissolutionThe resulting crude product is dissolved in 50 ml of ethyl acetate
  3. washwashed twice with 25 ml of water
  4. extractionthe organic extract
  5. dry with materialis dried over magnesium sulphate
  6. concentrationconcentrated under reduced pressure
  7. distillationThe crude product is distilled under reduced pressure

출처 및 근거

ORD 기록
ord-b947884471ff43dea42884fb63629a10
출처 데이터셋
uspto-grants-1993_09
특허 번호
US05243062

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