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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Water → HCID 21537737, 화합물

HRID 1076611
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HRID 1076611 반응식
[C:1]([NH:4][C:5]1[S:6][CH:7]=[C:8]([CH3:19])[C:9]=1[C:10](=[O:18])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[Cl:17])(=[O:3])[CH3:2].[H-].[Na+].[CH3:22]I.O>CN(C)C=O>[CH3:22][CH2:2][C:1]([NH:4][C:5]1[S:6][CH:7]=[C:8]([CH3:19])[C:9]=1[C:10](=[O:18])[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[Cl:17])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21537730HCID 21537730, 화합물

생성물 1

HCID 21537737HCID 21537737, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

To a solution of 40.0 g of 2-acetylamino-3-(o-chlorobenzoyl)-4-methylthiophene in 800 ml of dimethylformamide is added 7.74 g of 63 % sodium hydride. The mixture is stirred at room temperature for 30 minutes. Then 61.34 g of methyl iodide in 184 ml of dimethylformamide is added thereto. The mixture is stirred at room temperature for 2 hours, then poured into water, and extracted with benzene. The benzene extracts are washed with water, dried over sodium sulfate, and the solvent is removed under reduced pressure. The residual oil is chromatographed on silica gel, using chloroform as an eluent to give 2-(N-methylacetylamino)-3-(o-chlorobenzoyl)-4-methylthiophene as an oil.

후처리

  1. stirringThe mixture is stirred at room temperature for 2 hours
  2. extractionextracted with benzene
  3. washThe benzene extracts are washed with water
  4. dry with materialdried over sodium sulfate
  5. customthe solvent is removed under reduced pressure
  6. customThe residual oil is chromatographed on silica gel

출처 및 근거

ORD 기록
ord-393b181abd654a7c98c61536ae9a75b4
출처 데이터셋
uspto-grants-1976_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03957783

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