Chloroacetyl chloride → (S)-2-Chloro-N-(2,3-dihydroxypropyl)acetamide
反応式
C(N(CC)CC)C.[NH2:8][CH2:9][C@H:10]([OH:13])[CH2:11][OH:12].[Cl:14][CH2:15][C:16](Cl)=[O:17]>CC#N.CO>[Cl:14][CH2:15][C:16]([NH:8][CH2:9][C@H:10]([OH:13])[CH2:11][OH:12])=[O:17]参加物
5
実験手順
Triethylamine (4.0 ml, 28.9 mmol) was added to a solution of (S)-3-amino-1,2-propanediol (2.2 g, 24.1 mmol) in a mixture of CH3CN/MeOH (80 mL/13 mL) at −10° C. under nitrogen. Chloroacetyl chloride (2.1 mL, 26.5 mmol) was then added dropwise at −10° C. over 30 min. The reaction mixture was allowed to reach room temperature and stirred for 16 h. The mixture was concentrated under vacuum and purified by flash column chromatography on silica gel, eluting with methanol/ethyl acetate (8/92), to give the title compound as a white solid (3.63 g, 90%).
後処理
- customto reach room temperature
- concentrationThe mixture was concentrated under vacuum
- custompurified by flash column chromatography on silica gel
- washeluting with methanol/ethyl acetate (8/92)
出典と根拠
- ORDレコード
- ord-bdcb195f63e64282909f4dfe884f2e9e
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08058045B2
反応ノート
読み込み中…