HRID916776

反应详情

EQUATION

反应方程式

HRID 916776 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(Bromomethyl)cyclopropane (7.6 mL, 78 mmol) was added to a solution of 4-Chloro-7H-pyrrolo[2,3-d]pyrimidine (10.0 g, 65 mmol) and cesium carbonate (25.4 g, 78 mmol) in DMF (100 mL). The reaction mixture was stirred at room temperature 12 h, filtered, and concentrated in vacuo. Purification by flash column chromatography (silica, 1:9→2:8 EtOAc:hexanes) provided the title compound as a white solid (12.9 g, 95%). MS: 208.5 (MH+); HPLC Rf: 5.21 min. (HPLC method 4); HPLC purity: 100%.

WORKUP

后处理

  1. filtrationfiltered
  2. concentrationconcentrated in vacuo
  3. customPurification by flash column chromatography (silica, 1:9→2:8 EtOAc:hexanes)