HRID2039493

反应详情

EQUATION

反应方程式

HRID 2039493 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

250 mg (0.8 mmol) of the compound from Example 12A, 158 mg (1.0 mmol) of 4,4-difluoropiperidine hydrochloride and 435 μl (323 mg, 2.5 mmol) of N-ethyl-N-(propan-2-yl)propane-2-amine are initially charged in 5 ml of tetrahydrofuran and reacted in a single mode microwave (Emrys Optimizer) at 120° C. for 30 min. After pre-purification by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient), the product is additionally purified by column chromatography on silica gel (mobile phase dichloromethane/methanol, 10/1). Yield: 29 mg (10% of theory)

WORKUP

后处理

  1. customreacted in a single mode microwave (Emrys Optimizer) at 120° C. for 30 min
  2. customAfter pre-purification by preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient)
  3. customthe product is additionally purified by column chromatography on silica gel (mobile phase dichloromethane/methanol, 10/1)