HRID847623

反应详情

EQUATION

反应方程式

HRID 847623 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 22 mg of the resultant compound of Example 70 in 1 ml of dichloromethane was treated with 0.07 ml of ethyldiisopropylamine and 0.03 ml of chloromethyl methyl ether. The resulting solution was heated at reflux for 1 h. The cooled solution was concentrated in vacuo to give 26 mg of a crude solid which was recrystallized from ethyl acetate/chloroform to provide 15 mg of the desired compound (Rf 0.6, 10% methanol in chloroform) as a white solid, m.p. 197°-198° C. Mass spectrum: (M+H)+ =781.

WORKUP

后处理

  1. temperatureThe resulting solution was heated
  2. temperatureat reflux for 1 h
  3. concentrationThe cooled solution was concentrated in vacuo
  4. customto give 26 mg of a crude solid which
  5. customwas recrystallized from ethyl acetate/chloroform