Potassium Carbonate → 2-Cyano-3-(dimethoxythiophosphoryloxy)-5-methyl-thiophene

HRID 263025

반응식

HRID 263025 반응식
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:11][CH3:12])([O:9][CH3:10])=[S:8].[C:14]([C:16]1[S:17][C:18]([CH3:22])=[CH:19][C:20]=1[OH:21])#[N:15]>CC(C)=O>[C:14]([C:16]1[S:17][C:18]([CH3:22])=[CH:19][C:20]=1[O:21][P:7]([O:11][CH3:12])([O:9][CH3:10])=[S:8])#[N:15]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 17304Dimethyl phosphorochloridothionateHCID 213179292-Cyano-3-hydroxy-5-methyl-thiophene

생성물 1

HCID 540307152-Cyano-3-(dimethoxythiophosphoryloxy)-5-methyl-thiophene수율 89.1%

시약·촉매·용매 1

HCID 180Acetone용매

반응 조건

온도
20 °C

실험 절차

11.2 g of potassium carbonate and 12.8 g of O,O-dimethyl chlorothiophosphate were added to a solution of 11.2 g of 2-cyano-3-hydroxy-5-methyl-thiophene in 200 ml of acetone and the mixture was stirred for 15 hours at 20° C. and was then filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with a 7-3 cyclohexane-ethyl acetate mixture yielded 18.7 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-methyl-thiophene with a refractive index of nD20 =1.539.

후처리

  1. filtrationwas then filtered
  2. customThe filtrate was evaporated to dryness
  3. customthe residue was chromatographed over silica gel
  4. washElution with a 7-3 cyclohexane-ethyl acetate mixture

출처 및 근거

ORD 기록
ord-a78f1a106d41478e9c1abd56142ea0bb
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04155996

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