HRID379091

反应详情

EQUATION

反应方程式

HRID 379091 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-Methyl ethylenediamine (15 g, 202.3 mmol) was added dropwise to a stirred solution of ethyl trifluoroacetate (28.7 g, 204.34 mmol) in dry Et2O (50 mL) at 0° C. The resulting solution was stirred at room temperature for 2 hours. Hexane (75 mL) was added and the solution was left at −20° C. for 16 hours to produce a white precipitate which was removed by filtration, washed with Et2O (100 mL) and dried in vacuo for 3 hours to afford the title compound (29.4 g, 85%). 1H NMR (300 MHz, CDCl3) δ 3.42 (t, J=5.8 Hz, 2H), 2.80 (t, J=5.9 Hz, 2H), 2.43 (s, 3H); mass spectrum (API-TIS) 171 (M+H).

WORKUP

后处理

  1. waitthe solution was left at −20° C. for 16 hours
  2. customto produce a white precipitate which
  3. customwas removed by filtration
  4. washwashed with Et2O (100 mL)
  5. customdried in vacuo for 3 hours