Methanol → (S)-6-(Hydroxymethyl)morpholin-3-one
반응식
Cl[CH2:2][C:3]([NH:5][CH2:6][C@H:7]([OH:10])[CH2:8][OH:9])=[O:4].CC(C)([O-])C.[K+].CO.O>C(O)(CC)(C)C>[OH:9][CH2:8][C@@H:7]1[CH2:6][NH:5][C:3](=[O:4])[CH2:2][O:10]1참가 물질
6
실험 절차
(S)-2-Chloro-N-(2,3-dihydroxypropyl)acetamide (4.77 g, 28.45 mmol) in tert-amyl alcohol (75 mL) was added over 2 h to a stirred solution of potassium tert-butoxide (3.59 g, 21.4 mmol) in tert-amyl alcohol (25 mL) at room temperature under nitrogen. After 1 hr, methanol (12 mL) and water (0.7 mL) were added and the reaction mixture was stirred for an additional 20 min. The mixture was concentrated under vacuum and purified by flash column chromatography on silica gel, eluting with methanol/ethyl acetate (2/8), to give the title compound as a white solid (1.26 g, 45%).
후처리
- concentrationThe mixture was concentrated under vacuum
- custompurified by flash column chromatography on silica gel
- washeluting with methanol/ethyl acetate (2/8)
출처 및 근거
- ORD 기록
- ord-11bd976c6e7c45ee9bad9c13f57e501a
- 출처 데이터셋
- uspto-grants-2013_02
- 특허 번호
- US08367658B2
반응 노트
불러오는 중…