HRID626530
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
- 0 °C
PROCEDURE
实验过程
A 0° C. solution of methyl 1-hydroxycyclopropane-1-carboxylate (1 g, 8.61 mmol) in DMF (10 mL) was treated with NaH (60% in mineral oil, 0.689 g, 17.22 mmol), stirred at 0° C. for 0.5 h, treated with iodomethane (0.646 mL, 10.33 mmol), allowed to slowly warm to RT and stirred for 2 h. The mixture was quenched with satd. NH4Cl, diluted with water and extracted with Et2O (3×). The combined organics were washed with water, then brine, dried and concentrated to afford methyl 1-methoxycyclopropane-1-carboxylate (1.10 g, 98%). 1H NMR (400 MHz, DMSO-d6): δ 3.62 (s, 3H), 3.27 (s, 3H), 1.12-1.11 (m, 4H).
WORKUP
后处理
- temperatureto slowly warm to RT
- stirringstirred for 2 h
- customThe mixture was quenched with satd
- additionNH4Cl, diluted with water
- extractionextracted with Et2O (3×)
- washThe combined organics were washed with water
- dry with materialbrine, dried
- concentrationconcentrated