Potassium Carbonate → HCID 18415768、化合物

HRID 991001ノート

反応式

HRID 991001 の反応式
[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

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 696322-BromoacetamideHCID 135512470HCID 135512470、化合物

生成物 1

HCID 18415768HCID 18415768、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b03e9e334f874791a261999fd7aa6944
出典データセット
uspto-grants-2002_10
特許番号
US06462036B1

反応ノート

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