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Potassium Carbonate → HCID 19024816、化合物

HRID 249172
ノート
印刷プレビュー

反応式

HRID 249172 の反応式
[OH:1][C:2]1[CH:26]=[CH:25][C:5]([C:6]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[N:10]([CH2:17][CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH:9]=2)=[O:7])=[CH:4][CH:3]=1.Br[CH:28]([C:33]1[CH:38]=[CH:37][C:36]([CH2:39][CH:40]([CH3:42])[CH3:41])=[CH:35][CH:34]=1)[C:29]([CH3:32])([CH3:31])[CH3:30].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:30][C:29]([CH3:31])([CH3:32])[CH:28]([C:33]1[CH:34]=[CH:35][C:36]([CH2:39][CH:40]([CH3:41])[CH3:42])=[CH:37][CH:38]=1)[O:1][C:2]1[CH:26]=[CH:25][C:5]([C:6]([C:8]2[C:16]3[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=3)[N:10]([CH2:17][CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH:9]=2)=[O:7])=[CH:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 10871843Ethyl 4-[3-(4-hydroxybenzoyl)indol-1-yl]butyrateHCID 19024800HCID 19024800、化合物

生成物 1

HCID 19024816HCID 19024816、化合物収率 47.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A mixture of ethyl 4-[3-(4-hydroxybenzoyl)indol-1-yl]butyrate (0.50 g), 1-bromo-2,2-dimethyl-1-(4isobutylphenyl)propane (0.74 g) and potassium carbonate (0.59 g) in N,N-dimethylformamide (10 ml) was stirred at 60° C. for 20 hours. The reaction mixture was filtered, and the filtrate was poured into a mixture of ethyl acetate and 0.5N hydrochloric acid. The organic layer was separated, washed with water, and dried over magnesium sulfate. After evaporation of the solvent, the residue was purified by column chromatography on silica gel eluting a mixture of n-hexane and ethyl acetate (5:1) to give ethyl 4-[3-[4-[2,2-dimethyl-1-(4-isobutylphenyl)propyloxy]benzoyl]indol-1-yl]butyrate (376 mg) as an oil.

後処理

  1. filtrationThe reaction mixture was filtered
  2. additionthe filtrate was poured into a mixture of ethyl acetate and 0.5N hydrochloric acid
  3. customThe organic layer was separated
  4. washwashed with water
  5. dry with materialdried over magnesium sulfate
  6. customAfter evaporation of the solvent
  7. customthe residue was purified by column chromatography on silica gel eluting
  8. additiona mixture of n-hexane and ethyl acetate (5:1)

出典と根拠

ORDレコード
ord-03708194ed0c4ec49294dd4063a6f255
出典データセット
uspto-grants-1993_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05212320

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート