HRID1180381

反应详情

EQUATION

反应方程式

HRID 1180381 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Tert-butyl 4-{4-[(1-{[(cyanomethyl)amino]carbonyl}-3-methylbutoxy)(phenyl)methyl]benzoyl}piperazine-1-carboxylate from step 6 (0.09 g, 0.16 mmol) was dissolved in formic acid (1 mL). The mixture was aged for 2 hours and evaporated under reduced pressure. The crude residue was neutralized using a saturated aqueous solution of NaHCO3. The mixture was extracted 3 times with dichloromethane and the organic layers were dried and evaporated. The crude product was chromatographed on silica gel using 1% NH4OH and 9% methanol in dichloromethane to afford the title compound as a white solid.

WORKUP

后处理

  1. customevaporated under reduced pressure
  2. extractionThe mixture was extracted 3 times with dichloromethane
  3. customthe organic layers were dried
  4. customevaporated
  5. customThe crude product was chromatographed on silica gel using 1% NH4OH and 9% methanol in dichloromethane