HRID1084468

反应详情

EQUATION

反应方程式

HRID 1084468 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 0.433 g (0.0033 mol) of 4-chloro-2-oxo-2H-pyran and 0.41 g (0.0033 mol) of benzyl mercaptan in 2 ml of dimethyl formamide is added 0.228 g (0.00165 mol) of K2CO3. The reaction mixture is stirred for 1 hour and then the same amount of K2CO3 is once more added. The reaction mixture is then stirred overnight at 25° C., diluted with 30 ml of CH2C2, and extracted with 5×50 ml of a saturated aqueous solution of NaCl. The organic phase is dried over Na2SO4 and concentrated in a water jet vacuum. The distillation residue is chromatographed over silica gel. Yield: 0.36 g (50%). Melting point: 105°-106° C.

WORKUP

后处理

  1. stirringThe reaction mixture is then stirred overnight at 25° C.
  2. additiondiluted with 30 ml of CH2C2
  3. extractionextracted with 5×50 ml of a saturated aqueous solution of NaCl
  4. dry with materialThe organic phase is dried over Na2SO4
  5. concentrationconcentrated in a water jet vacuum
  6. distillationThe distillation residue is chromatographed over silica gel