Thionyl Chloride → 3-chlorocarbonyl-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole hydrochloride

HRID 1869175

反応式

HRID 1869175 の反応式
S(Cl)([Cl:3])=O.[C:5]([C:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]([C:17]2[C:18]3[CH:25]=[CH:24][N:23]([CH3:26])[C:19]=3[N:20]=[CH:21][N:22]=2)[CH:9]=1)(O)=[O:6]>>[ClH:3].[Cl:3][C:5]([C:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[N:10]([C:17]2[C:18]3[CH:25]=[CH:24][N:23]([CH3:26])[C:19]=3[N:20]=[CH:21][N:22]=2)[CH:9]=1)=[O:6]

参加物

3

反応物 2

HCID 24386Thionyl ChlorideHCID 689701693-carboxy-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole

生成物 1

HCID 865948063-chlorocarbonyl-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole hydrochloride

実験手順

6 cm3 of thionyl chloride are added to 0.9 g (3.08 mmol) of 3-carboxy-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole at a temperature in the region of 20° C. under an argon atmosphere. After stirring under reflux for 2 hours, the reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa), triturated twice successively with 30 cm3 of dichloromethane and then concentrated to dryness under reduced pressure (2.7 kPa), giving 0.92 g of 3-chlorocarbonyl-1-(7-methyl-7H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-indole hydrochloride in the form of a yellow powder, which is used directly in the following step.

後処理

  1. temperatureunder reflux for 2 hours
  2. concentrationthe reaction mixture is concentrated to dryness under reduced pressure (2.7 kPa)
  3. customtriturated twice successively with 30 cm3 of dichloromethane
  4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)

出典と根拠

ORDレコード
ord-d6a295153bca46af8eb415efc96077d1
出典データセット
uspto-grants-2009_12
特許番号
US07638521B2

関連ノート

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