HRID45984

反应详情

EQUATION

反应方程式

HRID 45984 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
44 °C

PROCEDURE

实验过程

(−)-(4-Chloro-phenyl)-(R)-(3-trifluoromethyl-phenoxy)-acetic acid 2-acetylamino-ethyl ester (90.0 g) was dissolved in diisopropylether (900 mL) at 55° C. The resulting mixture was polish filtered, the solution cooled to 44° C. over about 20 minutes and seeded. The resulting mixture was stirred for 1 hour at 44° C., cooled to 35° C. over 4 hours, then stirred at 35° C. for 2 hours to yield a thick suspension. The suspension was cooled to −5° C. over about 5 hours and then stirred at −5° C. The resulting crystals were filtered off with a centrifuge and washed with precooled (−5° C.) diisopropylether (100 mL). The wet product was dried at 30° C. to yield the title compound as a white crystalline solid, more specifically as white crystals, needles.

WORKUP

后处理

  1. filtrationfiltered
  2. temperaturecooled to 35° C. over 4 hours
  3. stirringstirred at 35° C. for 2 hours
  4. customto yield a thick suspension
  5. temperatureThe suspension was cooled to −5° C. over about 5 hours
  6. stirringstirred at −5° C
  7. filtrationThe resulting crystals were filtered off with a centrifuge
  8. washwashed with precooled (−5° C.) diisopropylether (100 mL)
  9. customThe wet product was dried at 30° C.