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

HRID 400464노트

반응식

HRID 400464 반응식
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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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

후처리

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

출처 및 근거

ORD 기록
ord-6d50818a27d4421b9ef657a436f1ce91
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08741892B2

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