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

HRID 263025

反応式

HRID 263025 の反応式
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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a78f1a106d41478e9c1abd56142ea0bb
出典データセット
uspto-grants-1979_05
特許番号
US04155996

関連ノート

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