HRID1180378

反应详情

EQUATION

反应方程式

HRID 1180378 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 tert-butyl 4-{4-[hydroxy(phenyl)methyl]benzoyl}piperazine-1-carboxylate from step 3 (1.5 g, 3.8 mmol) in DMF (20 mL) at 0° C. was added sodium hydride (0.16 g, 4.0 mmol) portionwise. The mixture was aged 15 minutes under a nitrogen atmosphere and methyl 2-bromo-4-methylpentanoate (0.65 mL, 4.0 mmol) was added dropwise. The reaction was allowed to warm to room temperature and was aged for 3 hours. The mixture was then partitioned between ethyl acetate and brine and the organic layer was dried and evaporated. The crude product was chromatographed on silica gel using 40% ethyl acetate in hexanes to afford the title compound.

WORKUP

后处理

  1. waitwas aged for 3 hours
  2. customThe mixture was then partitioned between ethyl acetate and brine
  3. customthe organic layer was dried
  4. customevaporated
  5. customThe crude product was chromatographed on silica gel using 40% ethyl acetate in hexanes