HRID979411

反应详情

EQUATION

反应方程式

HRID 979411 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

140 mg (1.1 mmol) of N-hydroxypyridine-2-thione in 5 ml of benzene are added dropwise at room temperature under an atmosphere of nitrogen to a solution of 120 mg (1.2 mmol) of phosgene in 5 ml of benzene, and this leads to the instantaneous precipitation of a white solid. 286 mg (1 mmol) of stearic acid and 0.5 ml of pyridine are added in 5 ml of benzene, and the reaction medium is taken to reflux for 4 hours. 3 mmol of tri-n-butylstannane in 5 ml of benzene with 10 mg of AIBN are added to the reaction medium during 10 minutes and refluxing is maintained for 2 and half hours. The reaction is carried out in the presence of tetrachloromethane, iodine and potassium fluoride, as indicated earlier. By filtration on silica (100% pentane), 168 mg of n-heptadecane are obtained. Yield 70%.

WORKUP

后处理

  1. customthis leads to the instantaneous precipitation of a white solid
  2. temperatureto reflux for 4 hours
  3. temperaturerefluxing
  4. temperatureis maintained for 2 and half hours
  5. filtrationBy filtration on silica (100% pentane), 168 mg of n-heptadecane
  6. customare obtained