HRID2257811

反应详情

EQUATION

反应方程式

HRID 2257811 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-40 °C

PROCEDURE

实验过程

To a solution of 0.20 g (1.42 mmol) of 3-(2-hydroxyethyl)-2-fluoropyridine in 8 ml of dry CH2Cl2 cooled to -40° C. was added 0.18 ml (0.8 mmol) trifluoromethanesulfonic anhydride under an atmosphere of nitrogen. After stirring for 30 min at -40° C., 30 ml of cold (-78° C.) NH3 (l) was added. The mixture was stirred for 30 min at -40° C., and then concentrated in vacuo to afford 1.03 g of crude salt which was washed twice with 20 ml diethyl ether to yield 0.82 g of 3-(2-aminoethyl)-2-fluoropyridine as a trifluoromethanesulfonic acid salt.

WORKUP

后处理

  1. stirringThe mixture was stirred for 30 min at -40° C.
  2. concentrationconcentrated in vacuo
  3. customto afford 1.03 g of crude salt which
  4. washwas washed twice with 20 ml diethyl ether