Hydroxyamine hydrochloride → HCID 6400952, 화합물
반응식
Cl.[NH2:2][OH:3].[CH3:4][NH:5][C:6](=[O:15])[C:7](=O)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>N1C=CC=CC=1>[OH:3][N:2]=[C:7]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:6]([NH:5][CH3:4])=[O:15]참가 물질
4
실험 절차
Hydroxylamine hydrochloride (5.96 g, 2.5 eq.) was added to a solution of N-methyl-2-oxo-2-phenylacetamide (5.6 g, 34.3 mmol) in pyridine (25 ml). After stirring for 10 h at room temperature, the excess pyridine was removed in vacuo and the residue was taken up in 250 ml of dichloromethane. The organic phase was washed with 200 ml of water and then again with aqueous hydrochloric acid (0.1 M, 250 ml). The precipitated solid was filtered off, giving 2-(hydroxyimino)-N-methyl-2-phenylacetamide as a yellow solid (2.31 g, pure Z isomer). The filtrate was concentrated by evaporation in vacuo. This gave 4.50 g of 2-(hydroxyimino)-N-methyl-2-phenylacetamide (Z/E=mixture of isomers) as a yellow solid.
후처리
- customthe excess pyridine was removed in vacuo
- washThe organic phase was washed with 200 ml of water
- filtrationThe precipitated solid was filtered off
출처 및 근거
- ORD 기록
- ord-3a6b693839be4a0aaf45d529f4caa07e
- 출처 데이터셋
- uspto-grants-2014_03
- 특허 번호
- US08680283B2
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