HRID500097

反应详情

EQUATION

反应方程式

HRID 500097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 4-(trifluoromethylthio)phenylhydrazine (1 g) in acetic acid (40 ml) was added 5-methyl-6-oxoheptane-1-sulphonic acid (1.4 g) and the solution heated to reflux overnight. The volatiles were removed on a rotary evaporator to give the crude product, 1.1 g of which was purified by preparative HPLC. The relevant fractions were combined, concentrated on a rotary evaporator and freeze dried to give the desired product (260 mg). M+=381

WORKUP

后处理

  1. temperaturethe solution heated
  2. temperatureto reflux overnight
  3. customThe volatiles were removed on a rotary evaporator
  4. customto give the crude product, 1.1 g of which
  5. customwas purified by preparative HPLC
  6. concentrationconcentrated on a rotary evaporator and freeze
  7. customdried