HRID927406
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-Amino-3-methyl-1-morpholinobutan-1-one (0.55 g, 2.96 mmol) and borane in THF (1 M, 6 mL, 6 mmol) were mixed together. The mixture was stirred at room temperature overnight, another portion borane in THF (6 mL) was added and the mixture stirred for another day. Methanol (5 mL) was added and the solvent was removed in vacuo. Water (20 mL) was added and the mixture was extracted with ethyl acetate (3×20 mL). The LC-MS showed still product in the water phase which was now extracted with methylene chloride (2×20 mL). The organic phases were combined, dried over anhydrous sodium sulfate and the solvent was removed in vacuo to give the crude product (0.09 g); MS (EI): m/e=173.2 [M+H]+.
WORKUP
后处理
- stirringthe mixture stirred for another day
- customthe solvent was removed in vacuo
- additionWater (20 mL) was added
- extractionthe mixture was extracted with ethyl acetate (3×20 mL)
- extractionwas now extracted with methylene chloride (2×20 mL)
- dry with materialdried over anhydrous sodium sulfate
- customthe solvent was removed in vacuo