HRID1947676

反应详情

EQUATION

反应方程式

HRID 1947676 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4-methyl-2-oxovaleric acid (8.07 mg; 0.062 mmol) was treated sequentially with 1-hydroxybenzotriazole hydrate (11.4 mg; 0.0741 mmol), EDC (14.3 mg; 0.074 mmol) and 1 1-[4-(methylsulfonyl)phenyl]-4,4′-bipiperidine (20.0.0 mg; 0.062 mmol) and stirred at ambient temperature for 18 h. The reaction was diluted with CH2Cl2(10 mL) and washed with water (15 mL). The organic phase was then dried over Na2SO4, filtered and concentrated in. vac to a residue. The crude product was purified by preparative HPLC reserve phase and eluted with acetonitrile/water+0.1% TFA. The title compound was isolated.

WORKUP

后处理

  1. washwashed with water (15 mL)
  2. dry with materialThe organic phase was then dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in
  5. customThe crude product was purified by preparative HPLC reserve phase
  6. washeluted with acetonitrile/water+0.1% TFA