Water → Ethyl 4,6-dichloro-3-formyl-1-[(4-methylphenyl)sulfonyl]-1H-indole-2-carboxylate

HRID 568186

反応式

HRID 568186 の反応式
[CH:1]([C:3]1[C:11]2[C:6](=[CH:7][C:8]([Cl:13])=[CH:9][C:10]=2[Cl:12])[NH:5][C:4]=1[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:2].C(=O)([O-])[O-].[K+].[K+].[C:25]1([CH3:35])[CH:30]=[CH:29][C:28]([S:31](Cl)(=[O:33])=[O:32])=[CH:27][CH:26]=1.O>CN(C)C=O>[CH:1]([C:3]1[C:11]2[C:6](=[CH:7][C:8]([Cl:13])=[CH:9][C:10]=2[Cl:12])[N:5]([S:31]([C:28]2[CH:29]=[CH:30][C:25]([CH3:35])=[CH:26][CH:27]=2)(=[O:33])=[O:32])[C:4]=1[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[O:2]

参加物

6

反応物 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 11430Potassium CarbonateHCID 2794948ethyl 4,6-dichloro-3-formyl-1H-indole-2-carboxylate

生成物 1

HCID 11305239Ethyl 4,6-dichloro-3-formyl-1-[(4-methylphenyl)sulfonyl]-1H-indole-2-carboxylate

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Combine 3-formyl-2-carboethoxy-4,6-dichloroindole (46.3 g. 162 mmol) and anhydrous potassium carbonate (44.9 g, 325 mmol) in dimethylformamide (600 mL). Add p-toluenesulfonyl chloride (42.9 g, 225 mmol). After 18 hours, pour the reaction mixture into water (3 L) and stir to give a solid. Filter, rinse with water and diethyl ether, and recrystallize from acetonitrile/dichloroethane to give the title compound.

後処理

  1. customto give a solid
  2. filtrationFilter
  3. washrinse with water and diethyl ether
  4. customrecrystallize from acetonitrile/dichloroethane

出典と根拠

ORDレコード
ord-9bc186136496456fa7a55e791b533f2c
出典データセット
uspto-grants-2001_01
特許番号
US06180786B2

関連ノート

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