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

HRID 65589

反応式

HRID 65589 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]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[CH:19][C:20]=1[OH:21])#[N:15]>C(#N)C>[C:14]([C:16]1[S:17][C:18]([O:22][CH2:23][CH2:24][CH2:25][CH3:26])=[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 213179005-Butoxy-3-hydroxythiophene-2-carbonitrile

生成物 1

HCID 545276212-Cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene収率 68.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
20 °C

実験手順

7 g of potassium carbonate and 8 g of O,O-dimethyl chlorothiophosphate were added to a solution of 9.8 g of 2-cyano-3-hydroxy-5-n-butoxy-thiophene in 150 ml of acetonitrile and the mixture was stirred for 24 hours at 20° C. and was then filtered. The filtrate was evaporated to dryness and the residue was chromatographed over silica gel. Elution with benzene yielded 11 g of 2-cyano-3-(dimethoxythiophosphoryloxy)-5-n-butoxy-thiophene with a refractive index of nD20 = 1.5375.

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 benzene

出典と根拠

ORDレコード
ord-d5f22fac622f4f12bc67103271588dd4
出典データセット
uspto-grants-1978_12
特許番号
US04128562

関連ノート

読み込み中…