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

HRID 263026

反応式

HRID 263026 の反応式
C(=O)([O-])[O-].[K+].[K+].[P:7](Cl)([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8].[C:16]([C:18]1[S:19][C:20]([CH3:24])=[CH:21][C:22]=1[OH:23])#[N:17]>CC(C)=O>[C:16]([C:18]1[S:19][C:20]([CH3:24])=[CH:21][C:22]=1[O:23][P:7]([O:12][CH2:13][CH3:14])([O:9][CH2:10][CH3:11])=[S:8])#[N:17]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioateHCID 213179292-Cyano-3-hydroxy-5-methyl-thiophene

生成物 1

HCID 542460502-Cyano-3-(diethoxythiophosphoryloxy)-5-methyl-thiophene収率 76.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
20 °C

実験手順

7 g of potassium carbonate and 9.5 g of O,O-diethyl chlorothiophosphate were added to a solution of 7 g of 2-cyano-3-hydroxy-5-methyl-thiophene in 100 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 an 8-2 cyclohexane-ethyl acetate mixture yielded 11.2 g of 2-cyano-3-(diethoxythiophosphoryloxy)-5-methyl-thiophene with a refractive index of nD20 =1.534.

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 an 8-2 cyclohexane-ethyl acetate mixture

出典と根拠

ORDレコード
ord-01b6035c65ea4f1a9e8bb1f6daf14852
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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