HRID415447

反应详情

EQUATION

反应方程式

HRID 415447 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 5-fluoropyrimidine-2-carbonitrile (Method 6, 1.0 g, 8.1 mmol) in anhydrous THF at −78° C. was added a solution of DIBAL-H (8.1 mL) over a period of 20 minutes. The resulting mixture was stirred at this temperature for 2 hours whereupon MeOH was added. The solution was allowed to warm to room temperature whereupon a solution of conc. HCl was added. The resulting mixture was stirred for 2 hours at ambient temperature and the aqueous layer was washed with EtOAc (3×). The combined organic extracts were washed with brine and dried (MgSO4). Evaporation of the solvent afforded the titled compound (780 mg, 76%). MS: [M+H]+ 127.

WORKUP

后处理

  1. additionwas added
  2. additionwas added
  3. washthe aqueous layer was washed with EtOAc (3×)
  4. washThe combined organic extracts were washed with brine
  5. dry with materialdried (MgSO4)
  6. customEvaporation of the solvent