HRID78745
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
CONDITIONS
反应条件
- 温度
- -2.5 °C
PROCEDURE
实验过程
Ethyl-2-(4,5-dihydrofuran-3-yl)-2-oxoacetate (45 g) was dissolved in tetrahydrofuran (225 ml) and Methanol (45 ml). The reaction mass was cooled to −5 to 0° C. N-bromosuccinimide (47 g) was added lot wise by maintaining temp below 0° C. Reaction mass was then stirred at 20-25° C. for 12 hrs. Reaction mass was concentrated to residue under vacuum at 40° C. Residue was dissolved in Ethyl acetate (450 ml) and washed with sodium sulphite solution (10%, 2×135 ml). Reaction mass was then concentrated to residue to get ethyl-2-(3-bromo-2-methoxytetrahydrofuran-3-yl)-2-oxoacetate (Yield 63 g).
WORKUP
后处理
- temperatureby maintaining temp below 0° C
- customReaction mass
- customReaction mass
- concentrationwas concentrated to residue under vacuum at 40° C
- dissolutionResidue was dissolved in Ethyl acetate (450 ml)
- washwashed with sodium sulphite solution (10%, 2×135 ml)
- customReaction mass
- concentrationwas then concentrated to residue