Hydrochloric Acid → Awd 12-281

HRID 1265312

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HRID 1265312 반응식
[Cl-].[Al+3].[Cl-].[Cl-].S1C=CCS1.[Cl:10][C:11]1[CH:12]=[N:13][CH:14]=[C:15]([Cl:41])[C:16]=1[NH:17][C:18](=[O:40])[C:19]([C:21]1[C:29]2[C:24](=[CH:25][CH:26]=[C:27]([O:30]C)[CH:28]=2)[N:23]([CH2:32][C:33]2[CH:38]=[CH:37][C:36]([F:39])=[CH:35][CH:34]=2)[CH:22]=1)=[O:20].Cl>ClCCl>[Cl:10][C:11]1[CH:12]=[N:13][CH:14]=[C:15]([Cl:41])[C:16]=1[NH:17][C:18](=[O:40])[C:19]([C:21]1[C:29]2[C:24](=[CH:25][CH:26]=[C:27]([OH:30])[CH:28]=2)[N:23]([CH2:32][C:33]2[CH:38]=[CH:37][C:36]([F:39])=[CH:35][CH:34]=2)[CH:22]=1)=[O:20]

참가 물질

6

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온도
0 °C

실험 절차

5 g (38 mmol) anhydrous aluminium chloride is introduced into 50 ml ethane-1,2, -dithiol. A solution of 4.7 g of N-(3,5-dichloropyridin-4-yl)-2-[1-(4-fluorobenzyl)-5-methoxyindol-3-yl]-2-oxoacetamide (10 mmol) in 50 ml of dichloromethane is added at 0° C. The mixture is stirred at 0° C. for 4 hours. 50 ml of 10% hydrochloric acid is added dropwise at from 0 to 10° C. with stirring. The crystallizing product is isolated, washed with water and dried at 20° C. A pure product is obtained by recrystallization from ethanol (180 ml).

후처리

  1. stirringwith stirring
  2. customThe crystallizing product is isolated
  3. washwashed with water
  4. customdried at 20° C
  5. customA pure product is obtained by recrystallization from ethanol (180 ml)

출처 및 근거

ORD 기록
ord-5f8e1b377ea742c18e2495e1d3ae7d62
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06545158B2

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