HRID267352
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
A mixture of 40.0 g. (0.19 mole) of ethyl 4-bromo-2-methylbutyrate (Tetrahedron 21, 2966 (1965)), 66.0 g. (0.76 mole) of morpholine and 750 ml. of benzene was heated at 60°C. for 5 hours and stirred at room temperature for a total of 40 hours. A colorless solid was removed by filtration, and the mother liquor was evaporated to give a colorless, mobile residue. This material was combined with 250 ml. of ether and filtered to remove a small amount of additional solid. The solution was concentrated and the residue distilled to give the desired material as 38.0 g. (93%) of colorless liquid (b.p. 71°-73°C. at 0.10 mm).
WORKUP
后处理
- additionA mixture of 40.0 g
- customA colorless solid was removed by filtration
- customthe mother liquor was evaporated
- customto give a colorless, mobile residue
- filtrationof ether and filtered
- customto remove a small amount of additional solid
- concentrationThe solution was concentrated
- distillationthe residue distilled