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Potassium Hydroxide → HCID 21537722、化合物

HRID 1076612
ノート
印刷プレビュー

反応式

HRID 1076612 の反応式
CC[C:3]([NH:5][C:6]1[S:7][CH:8]=[C:9]([CH3:20])[C:10]=1[C:11](=[O:19])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18])=O.[OH-].[K+]>C(O)C.O>[CH3:3][NH:5][C:6]1[S:7][CH:8]=[C:9]([CH3:20])[C:10]=1[C:11](=[O:19])[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 21537737HCID 21537737、化合物

生成物 1

HCID 21537722HCID 21537722、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

反応条件

温度
95 °C

実験手順

To a solution of 29.6 g of 2-(N-methylacetylamino)-3-(o-chlorobenzoyl)-4-methylthiophene in 592 ml of ethanol, is added 6.97 g of potassium hydroxide in 190 ml of water. The mixture is heated at 95°C for 1 hour, evaporated under reduced pressure to a residue. Water is added to the residue and extracted with chloroform. The chloroform extracts are washed with water, dried over sodium sulfate, then evaporated under reduced pressure to give an oil. The residual oil is chromatographed on silica gel, using chloroform as an eluent to give 2-methylamino-3-(o-chlorobenzoyl)-4-methylthiophene as crystals having a melting point of 132° - 134°C (after recrystallization from ethanol).

後処理

  1. customevaporated under reduced pressure to a residue
  2. additionWater is added to the residue
  3. extractionextracted with chloroform
  4. washThe chloroform extracts are washed with water
  5. dry with materialdried over sodium sulfate
  6. customevaporated under reduced pressure
  7. customto give an oil
  8. customThe residual oil is chromatographed on silica gel

出典と根拠

ORDレコード
ord-05ba35e44a3a49c69de83505f297de46
出典データセット
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03957783

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート