Dimethylformamide → 1-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepine-4-carbaldehyde hydrochloride

HRID 400464ノート

反応式

HRID 400464 の反応式
O=P(Cl)(Cl)[Cl:3].CN([CH:9]=[O:10])C.[ClH:11].[CH2:12]([N:19]1[CH2:25][CH2:24][CH2:23][C:22](=O)[CH2:21][CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>ClCCl>[ClH:3].[CH2:12]([N:19]1[CH2:25][CH2:24][C:23]([Cl:11])=[C:22]([CH:9]=[O:10])[CH2:21][CH2:20]1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 130720291-Benzylazepan-4-one hydrochloride

生成物 1

HCID 189435411-benzyl-5-chloro-2,3,6,7-tetrahydro-1H-azepine-4-carbaldehyde hydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

77 mL phosphoroxychloride was added to 62 mL DMF at 8-18° C. 84 mL dichlormethane was added and 50 g 1-benzyl 4-azepanone hydrochloride. The reaction was stirred over night at RT. The mixture was added to 300 mL ice water and extracted with dichlormethane. The organic layer was evaporated to give 23.3 g of the desired product. (M+H)+=287

後処理

  1. extractionextracted with dichlormethane
  2. customThe organic layer was evaporated

出典と根拠

ORDレコード
ord-6d50818a27d4421b9ef657a436f1ce91
出典データセット
uspto-grants-2014_06
特許番号
US08741892B2

反応ノート

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