反应详情

To an ice water cooled solution of lithium aluminum hydride (200 mL of 1.0 M) was added solid 2(R)-amino-3-cyclopropylmethylsulfanylpropionic acid. The addition was done by tapping in portions through a funnel in such a manner as to control hydrogen gas evolution. The ice bath was removed, and the reaction mixture was heated at reflux for 16 h. The reaction mixture was removed from heat and cooled in an ice water bath. Diethyl ether (110 mL) was added, followed by dropwise addition of water (5 mL), 15% aqueous sodium hydroxide (5 mL), and water (15 mL). After stirring in the ice water bath for 1.5 h, the reaction mixture was filtered. The filtrate was dried over anhydrous sodium sulfate, and concentrated to give 2(R)-amino-3-cyclopropylmethylsulfanylpropan-1-ol (14.9 g).

1. additionThe addition
2. customby tapping in portions through a funnel
3. customThe ice bath was removed
4. temperaturethe reaction mixture was heated
5. temperatureat reflux for 16 h
6. customThe reaction mixture was removed
7. temperaturefrom heat
8. temperaturecooled in an ice water bath
9. additionDiethyl ether (110 mL) was added
10. additionfollowed by dropwise addition of water (5 mL), 15% aqueous sodium hydroxide (5 mL), and water (15 mL)
11. filtrationthe reaction mixture was filtered
12. dry with materialThe filtrate was dried over anhydrous sodium sulfate
13. concentrationconcentrated