HRID842600

反应详情

EQUATION

反应方程式

HRID 842600 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2.56 mmol of 6-[(triphenylmethyl)thio]-1,3,3,-hexanetricarboxylic acid (III) (1.36 g) was dissolved in 5 ml of dimethylsulfoxide and the solution was ad heated to 100° C. for 1 hour, evaporated to dryness, dissolved in water and precipitated by addition of 1 M sulfuric acid. The precipitated oil solidified after 1 hour treatment in an ultrasound bath. The solid was filtered off, washed with water and dried in a dessicator. Yield 1.1 g of 6-[(triphenylmethyl)thio]-1,3-hexanedicarboxylic acid (IV) (89% two steps from II), 13C-NMR (MeOH) δ27.9, 28.6, 33.0 (two carbons), 33.1, 45.9, 68.1, 128.1, 129.2, 131.2, 146.8, 177.1, 179.4.

WORKUP

后处理

  1. customevaporated to dryness
  2. dissolutiondissolved in water
  3. customprecipitated by addition of 1 M sulfuric acid
  4. filtrationThe solid was filtered off
  5. washwashed with water
  6. customdried in a dessicator