HRID626530

反应详情

EQUATION

反应方程式

HRID 626530 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureto slowly warm to RT
  2. stirringstirred for 2 h
  3. customThe mixture was quenched with satd
  4. additionNH4Cl, diluted with water
  5. extractionextracted with Et2O (3×)
  6. washThe combined organics were washed with water
  7. dry with materialbrine, dried
  8. concentrationconcentrated