Triethylamine → Methyl (S)-2-methyl-3-((methylsulfonyl)oxy)propanoate
反応式
[OH:1][CH2:2][C@H:3]([CH3:8])[C:4]([O:6][CH3:7])=[O:5].[CH3:9][S:10](Cl)(=[O:12])=[O:11].CCN(CC)CC>C(Cl)Cl>[CH3:9][S:10]([O:1][CH2:2][C@H:3]([CH3:8])[C:4]([O:6][CH3:7])=[O:5])(=[O:12])=[O:11]参加物
5
実験手順
A solution of methyl 3-hydroxy-2-(S)-methylpropanoate (35 g, 295 mmol) in 830 mL of CH2Cl2, under N2 atmosphere, was cooled to -60° C. With rapid stirring, methanesulfonyl chloride (24 mL, 310 mmol) was added, followed by Et3N (50 mL, 354 mmol) over 90 s. As the addition ended, a heavy white precipitate formed which stopped the magnetic stirring. The cold bath was removed and the reaction allowed to reach r.t. The reaction mixture was poured into aq 25% NH4OAc. After separation, the organic phase was dried over MgSO4 and evaporated to give the title compound as a colorless oil (59.1 g, 102%).
後処理
- additionAs the addition
- customa heavy white precipitate formed which
- customThe cold bath was removed
- customto reach r.t
- additionThe reaction mixture was poured into aq 25% NH4OAc
- customAfter separation
- dry with materialthe organic phase was dried over MgSO4
- customevaporated
出典と根拠
- ORDレコード
- ord-1c77de2087dd4de8848a021796489ba1
- 出典データセット
- uspto-grants-1993_11
- 特許番号
- US05266568
反応ノート
読み込み中…