HRID244414

反应详情

EQUATION

反应方程式

HRID 244414 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 3-methyl-5-{2,2,2-trifluoro-1-[1-(4-fluorophenyl)-1H-indazol-5-yl]-1-hydroxyethyl}-1H-pyridin-2-one (0.184 mmol) in 1 mL DMF was added NaH (0.221 mmol; 60% suspension in oil) in several portions. After 1 hour, iodomethane (0.20 mmol) was added. After 1 hour, the mixture was diluted with water and the solid was collected by filtration, washed with water and dried. The residue was purified with flash silica gel chromatography using 25% hexanes in ethyl acetate. The product-rich fractions were concentrated in vacuo to provide the title compound (0.051 mmol), m.p.>200° C.

WORKUP

后处理

  1. waitAfter 1 hour
  2. filtrationthe solid was collected by filtration
  3. washwashed with water
  4. customdried
  5. customThe residue was purified with flash silica gel chromatography
  6. concentrationThe product-rich fractions were concentrated in vacuo