反应详情

A solution of methyl 3-methyl-N-{[methyl(pent-4-enyl)amino]carbonyl}-L-valinate (3.00 g, 11.2 mmol), lithium hydroxide (1M, 56.0 mL, 56.0 mmol) in tetrahydrofuran (40 mL) was heated to 50° C. for 1 h. Contents of the reaction flask were cooled and evaporated to remove tetrahydrofuran. The remaining mixture was poured into 5% potassium bisulfate and extracted with methylene chloride (3×10 mL). The combined organic extracts were dried with anhydrous sodium sulfate, filtered and evaporated to give the title compound as a colorless oil, 2.87 g (100% yield). LRMS (ESI) m/z 257 [(M+H)+; calcd for C13H25N2O3: 257].

1. temperatureContents of the reaction flask were cooled
2. customevaporated
3. customto remove tetrahydrofuran
4. additionThe remaining mixture was poured into 5% potassium bisulfate
5. extractionextracted with methylene chloride (3×10 mL)
6. dry with materialThe combined organic extracts were dried with anhydrous sodium sulfate
7. filtrationfiltered
8. customevaporated