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Potassium Hydroxide → HCID 21537722, 화합물

HRID 1076612
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HRID 1076612 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 21537737HCID 21537737, 화합물

생성물 1

HCID 21537722HCID 21537722, 화합물

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
95 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-05ba35e44a3a49c69de83505f297de46
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957783

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