HRID1295659

反应详情

EQUATION

反应方程式

HRID 1295659 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a suspension of 1.83 g of {4-[4-(benzo[1,3]dioxol-5-ylamino)-7H-pyrrolo[2,3-d]pyrimidin-6-yl ]-phenyl}-methanol in 56 ml of dioxane/acetonitrile 1:1 under N2-atmosphere, 3.1 ml of thionylchloride are added. After 16 h stirring, the suspension is diluted with ethyl acetate and NaHCO3-solution. The aqueous layer is separated off and extracted twice with ethyl acetate. The organic phases are washed with water and brine, dried (MgSO4) and concentrated to yield the title compound; MS-ES+: (M+H)+=379; HPLC (conditions see Examples 67-78) tR=11.4 min.

WORKUP

后处理

  1. customThe aqueous layer is separated off
  2. extractionextracted twice with ethyl acetate
  3. washThe organic phases are washed with water and brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated