Ethanol → 3-Amino-6-chloro-2-(3-methylbenzoyl)-1H-indole

HRID 651010

反応式

HRID 651010 の反応式
[NH2:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([Cl:11])=[CH:8][CH:9]=2)[N:4](C(OCC)=O)[C:3]=1[C:17](=[O:25])[C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[CH:19]=1.C([O-])([O-])=O.[K+].[K+].CCO>O>[NH2:1][C:2]1[C:10]2[C:5](=[CH:6][C:7]([Cl:11])=[CH:8][CH:9]=2)[NH:4][C:3]=1[C:17](=[O:25])[C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[CH:19]=1

参加物

5

反応物 3

HCID 702EthanolHCID 11430Potassium CarbonateHCID 183680433-Amino-6-chloro-2-(3-methylbenzoyl)-1-(ethoxycarbonyl)indole

生成物 1

HCID 183678773-Amino-6-chloro-2-(3-methylbenzoyl)-1H-indole収率 84%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of ethyl 3-amino-6-chloro2-(3-methylbenzoyl)-1H-indole-1-caboxylate (step 1, 6.4 g, 18 mmol), K2CO3 (6.3 g, 45 mnmol) , EtOH (50 ml) and water (30 ml) was heated at reflux temperature for 20 h. The mixture was concentrated, and then water (30 ml) was added to the residue. The resulting mixture was extracted with dichloromethane (80 ml×2) and the combined extracts were dried (MgSO4). Removal of solvent gave 4.3 g (84%) of brown amorphous solids.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 20 h
  3. concentrationThe mixture was concentrated
  4. additionwater (30 ml) was added to the residue
  5. extractionThe resulting mixture was extracted with dichloromethane (80 ml×2)
  6. dry with materialthe combined extracts were dried (MgSO4)
  7. customRemoval of solvent

出典と根拠

ORDレコード
ord-78ad45ccc9a54c70a1c8741eceb8479b
出典データセット
uspto-grants-2001_08
特許番号
US06277878B1

関連ノート

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