Methanesulfonic Acid → 2-[(Methanesulfonyl)oxy]butane-1,4-diyl dimethanesulfonate
反応式
[CH3:1][S:2]([OH:5])(=[O:4])=[O:3].C(N([CH2:11][CH3:12])CC)C>C(OCC)(=O)C>[CH3:1][S:2]([O:5][CH:11]([CH2:12][O:5][S:2]([CH3:1])(=[O:4])=[O:3])[CH2:12][CH2:11][O:5][S:2]([CH3:1])(=[O:4])=[O:3])(=[O:4])=[O:3]参加物
4
反応条件
- 温度
- 2.5 °C
実験手順
A solution of 18.1 ml of methanesulphonic acid in 45 ml of ethyl acetate was added dropwise within 2 hours under argon to a solution, cooled to 0-5° C., of 7.96 g of S-1,2,4-butanetriol and 33.5 ml of triethylamine in 90 ml of ethyl acetate. The white suspension was stirred at 0-5° C. for a further 2 hours and thereafter the suspension was filtered and the yellow filtrate was washed in succession with 75 ml of 1N hydrochloric acid, 75 ml of saturated NaHCO3 solution and 75ml of saturated NaCl solution. The organic phase was dried over Na2SO4, filtered and the filtrate was concentrated. 21.79 g of yellow oil were obtained.
後処理
- filtrationthe suspension was filtered
- washthe yellow filtrate was washed in succession with 75 ml of 1N hydrochloric acid, 75 ml of saturated NaHCO3 solution and 75ml of saturated NaCl solution
- dry with materialThe organic phase was dried over Na2SO4
- filtrationfiltered
- concentrationthe filtrate was concentrated
出典と根拠
- ORDレコード
- ord-d56c5b2b22de4731a6d947cd325624b1
- 出典データセット
- uspto-grants-1999_11
- 特許番号
- US05977381
反応ノート
読み込み中…