Methanol → (S)-6-(Hydroxymethyl)morpholin-3-one
反応式
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]1参加物
6
実験手順
(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%).
後処理
- concentrationThe mixture was concentrated under vacuum
- custompurified by flash column chromatography on silica gel
- washeluting with methanol/ethyl acetate (2/8)
出典と根拠
- ORDレコード
- ord-11bd976c6e7c45ee9bad9c13f57e501a
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08367658B2
反応ノート
読み込み中…