HRID1765542

反应详情

EQUATION

反应方程式

HRID 1765542 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Potassium t-butoxide (18.8 g) was added to a stirred solution of 2-chloro-5-iodo-N-(tricyclo [3.3.1.13,7]dec-1-ylmethyl)benzamide (prepared as described in WO 99/29661) (60.0 g) in anhydrous tetrahydrofuran (600 mL) at 20° C. under nitrogen. After the addition was complete, 4-methoxybenzyl chloride (20.8 mL) was added. The mixture was heated to reflux for 12 hours and then cooled to room temperature. Water (600 mL) was added and the mixture extracted with dichloromethane (1.2 L then 400 mL). Organic extracts were dried over anhydrous magnesium sulphate, filtered and evaporated under reduced pressure.

WORKUP

后处理

  1. additionAfter the addition
  2. temperatureThe mixture was heated
  3. temperatureto reflux for 12 hours
  4. extractionthe mixture extracted with dichloromethane (1.2 L
  5. dry with materialOrganic extracts were dried over anhydrous magnesium sulphate
  6. filtrationfiltered
  7. customevaporated under reduced pressure