HRID2053092

反应详情

EQUATION

反应方程式

HRID 2053092 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred suspension of sodium hydride (630 mg, 60% dispersion in mineral oil) in tetrahydrofuran (20 ml) at 0° C. was added benzyl alcohol (1.09 ml). The mixture was stirred for 15 minutes then a solution of 4-chloro-2-methylsulfanyl-6-(3-trifluoromethyl-phenyl)-pyrimidine (1.6 g) in tetrahydrofuran (14 ml) was added dropwise. The reaction was allowed to warm to room temperature and stirred for two hours. Solvent was evaporated under reduced pressure and the remaining residue dissolved in dichloromethane (200 ml) and washed with water (2×150 ml). Organics were separated, dried over sodium sulphate and solvent was removed under reduced pressure to yield crude product (2.5 g). Flash chromatography on silica yielded product 4-benzyloxy-2-methylsulfanyl-6-(3-trifluoromethyl-phenyl)-pyrimidine (1.75 g) as a yellow solid.

WORKUP

后处理

  1. stirringstirred for two hours
  2. customSolvent was evaporated under reduced pressure
  3. dissolutionthe remaining residue dissolved in dichloromethane (200 ml)
  4. washwashed with water (2×150 ml)
  5. customOrganics were separated
  6. dry with materialdried over sodium sulphate and solvent
  7. customwas removed under reduced pressure