HRID898594

反应详情

EQUATION

反应方程式

HRID 898594 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

0.141 mL (1.080 mmol) chloroformic acid-isopropylester was added dropwise at −10° C. to a solution of 0.254 g (0.982 mmol) (2-chloro-4-trifluoromethyl-phenoxy)-acetic acid (Z2b) and 0.119 mL (1.080 mmol) N-methylmorpholine in 20 mL abs. THF and the mixture was stirred for a further 10 min. 0.250 g (1.031 mmol) 2-chloro-4-(2-diethylamino-ethoxy)-phenylamine (Z27b) was added, the mixture was stirred for 1 h at RT and then evaporated down i. vac. Water was added and the aqueous phase was exhaustively extracted with dichloromethane. The combined org. phases were dried over sodium sulphate, evaporated down i. vac. and the residue stirred with ether. The precipitate was filtered off, washed with ether and dried in a HV.

WORKUP

后处理

  1. customevaporated down i
  2. additionWater was added
  3. extractionthe aqueous phase was exhaustively extracted with dichloromethane
  4. dry with materialphases were dried over sodium sulphate
  5. customevaporated down i
  6. stirringand the residue stirred with ether
  7. filtrationThe precipitate was filtered off
  8. washwashed with ether
  9. customdried in a HV