반응식
[CH2:1]([O:7][C:8]1[CH:13]=[CH:12][C:11]([S:14]([N:17]([CH2:24][CH:25]([CH3:27])[CH3:26])[CH2:18][C:19](OCC)=[O:20])(=[O:16])=[O:15])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6].Cl.[NH2:29][OH:30].C[O-].[Na+].[Na]>CO>[OH:30][NH:29][C:19](=[O:20])[CH2:18][N:17]([S:14]([C:11]1[CH:12]=[CH:13][C:8]([O:7][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH3:6])=[CH:9][CH:10]=1)(=[O:16])=[O:15])[CH2:24][CH:25]([CH3:27])[CH3:26]참가 물질
실험 절차
Ethyl 2-[[4-hexyloxybenzenesulfonyl](isobutyl)amino]acetate (1.22 g, 3.05 mmol) is dissolved in methanol (15 mL). To this solution is added hydroxylamine hydrochloride (0.43 g, 6.11 mmol), followed by the addition of sodium methoxide, freshly prepared from sodium (0.35 g, 15.3 mmol) dissolved in methanol (5 mL). The reaction is stirred for 36 hours at room temperature. The reaction is worked up by partitioning between dilute hydrochloric acid (pH=~3) and ethyl acetate. The aqueous phase is extracted well with ethyl acetate, the combined organic layers are dried (Na2SO4), and the solvent is evaporated. The product is crystallized from hexane/ethyl acetate and collected by filtration to give N-hydroxy-2-[[4-hexyloxybenzenesulfonyl](isobutyl)-amino]acetamide, m.p. 108°-110° C.
후처리
- customby partitioning between dilute hydrochloric acid (pH=~3) and ethyl acetate
- extractionThe aqueous phase is extracted well with ethyl acetate
- dry with materialthe combined organic layers are dried (Na2SO4)
- customthe solvent is evaporated
- customThe product is crystallized from hexane/ethyl acetate
- filtrationcollected by filtration
출처 및 근거
- ORD 기록
- ord-477f3476ce344ca290a646b1cb740e71
- 출처 데이터셋
- uspto-grants-1996_09
- 특허 번호
- US05552419
연결된 노트
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