Hydrochloric Acid → Awd 12-281

HRID 394572ノート

反応式

HRID 394572 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].C(S)CS.[Cl:9][C:10]1[CH:11]=[N:12][CH:13]=[C:14]([Cl:40])[C:15]=1[NH:16][C:17](=[O:39])[C:18]([C:20]1[C:28]2[C:23](=[CH:24][CH:25]=[C:26]([O:29]C)[CH:27]=2)[N:22]([CH2:31][C:32]2[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=2)[CH:21]=1)=[O:19].Cl>ClCCl>[Cl:9][C:10]1[CH:11]=[N:12][CH:13]=[C:14]([Cl:40])[C:15]=1[NH:16][C:17](=[O:39])[C:18]([C:20]1[C:28]2[C:23](=[CH:24][CH:25]=[C:26]([OH:29])[CH:27]=2)[N:22]([CH2:31][C:32]2[CH:37]=[CH:36][C:35]([F:38])=[CH:34][CH:33]=2)[CH:21]=1)=[O:19]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 109021,2-EthanedithiolHCID 6451240Aluminum(III) ChlorideHCID 11123551N-(3,5-dichloropyridin-4-yl)-2-[1-(4-fluorobenzyl)-5-methoxyindol-3-yl]-2-oxoacetamide

生成物 1

HCID 6918428Awd 12-281

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

5 g (38 mmol) anhydrous aluminium chloride is introduced into 50 ml ethane-1,2,-dithiol. A solution of 4.7 g of N-(3,5-dichloropyridin-4-yl)-2-[1-(4-fluorobenzyl)-5-methoxyindol-3-yl]-2-oxoacetamide (10 mmol) in 50 ml of dichloromethane is added at 0° C. The mixture is stirred at 0° C. for 4 hours. 50 ml of 10% hydrochloric acid is added dropwise at from 0 to 10° C. with stirring. The crystallizing product is isolated, washed with water and dried at 20° C. A pure product is obtained by recrystallization from ethanol (180 ml).

後処理

  1. stirringwith stirring
  2. customThe crystallizing product is isolated
  3. washwashed with water
  4. customdried at 20° C
  5. customA pure product is obtained by recrystallization from ethanol (180 ml)

出典と根拠

ORDレコード
ord-ed2391d4e4b94b39ba205b25ab1a6540
出典データセット
uspto-grants-2003_08
特許番号
US06602890B2

反応ノート

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