Potassium Carbonate → HCID 18415768, 화합물

HRID 991001노트

반응식

HRID 991001 반응식
[NH:1]1[C:5]2[C:6]3[C:11]([CH2:12][C:4]=2[C:3]([C:13]2[CH:18]=[CH:17][C:16]([OH:19])=[CH:15][CH:14]=2)=[N:2]1)=[CH:10][CH:9]=[CH:8][CH:7]=3.C(=O)([O-])[O-].[K+].[K+].Br[CH2:27][C:28]([NH2:30])=[O:29]>CN(C)C=O.ClCCl>[NH:1]1[C:5]2[C:6]3[C:11]([CH2:12][C:4]=2[C:3]([C:13]2[CH:18]=[CH:17][C:16]([O:19][CH2:27][C:28]([NH2:30])=[O:29])=[CH:15][CH:14]=2)=[N:2]1)=[CH:10][CH:9]=[CH:8][CH:7]=3

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 696322-BromoacetamideHCID 135512470HCID 135512470, 화합물

생성물 1

HCID 18415768HCID 18415768, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 6344Dichloromethane용매

실험 절차

A mixture of 4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)phenol (0.28 g, Example 30), potassium carbonate (0.16 g) and 2-bromoacetamide (0.16 g) was stirred together at ambient temperature in dry dimethyl formamide (5 ml) for 4 days and then allowed to stand at ambient temperature for 9 days. The mixture was diluted with dichloromethane (50 ml) and washed with 1M aqueous sodium hydroxide solution and then with water. Some insoluble material which remained throughout the extractions was collected by filtration. The solid was purified by flash column chromatography on silica using ethyl acetate as the mobile phase. Appropriate fractions were collected, combined and evaporated to give 2-[4-(1,4-dihydroindeno[1,2-c]pyrazol-3-yl)phenoxy]acetamide, m.p. 247-248° C.

후처리

  1. washwashed with 1M aqueous sodium hydroxide solution
  2. extractionSome insoluble material which remained throughout the extractions
  3. filtrationwas collected by filtration
  4. customThe solid was purified by flash column chromatography on silica
  5. customAppropriate fractions were collected
  6. customevaporated

출처 및 근거

ORD 기록
ord-b03e9e334f874791a261999fd7aa6944
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06462036B1

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