HRID1612570

反应详情

EQUATION

反应方程式

HRID 1612570 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

At 20° to 25° C. and over a period of 1 hour, 108 ml of triethylamine was dripped into a mixture of 165 g (0.71 mol) of 1-bromo-2-(2-fluorobenzyloxy)-ethane, 116 g (0.7 mol) of N-hydroxyphthalimide and 710 ml of N-methyl-2-pyrrolidone. After the mixture had been kept for 5 hours at 60° C., the cold mixture was poured into 2000 ml of ice water, the precipitate was suction filtered, washed with water and isopropanol and dried under reduced pressure over phosphorus pentoxide. There was obtained 185 g (82%) of phthalimide ether, m.p. 62°-64° C. 1H-NMR (250 MHZ, d6 -DMSO): δ=3.85 (m,2H), 4.35 (m,2H), 4.54 (s,2H), 7.10-7.40 (m,4H), 7.88 (s,4H).

WORKUP

后处理

  1. waitAfter the mixture had been kept for 5 hours at 60° C.
  2. filtrationfiltered
  3. washwashed with water and isopropanol
  4. dry with materialdried under reduced pressure over phosphorus pentoxide