HRID736343

反应详情

EQUATION

反应方程式

HRID 736343 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

2-Fluoro-benzenesulfonyl chloride (72 mg, 0.37 mmol) was added to a solution of (4-Amino-7-isopropyl-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-(6-amino-pyridin-2-yl)-methanone (100 mg 0.34 mmol) in pyridine (2 mL). The resulting solution was heated to 40° C. in a sealed tube for 12 h. The reaction mixture was concentrated in vacuo and the residue was triturated with MeOH and filtered to provide a crude yellow solid. Purification by flash column chromatography (hexanes/ethyl acetate 5:5-1:9) afforded the title compound as a yellow solid (60 mg, 40%). MS: 455.1 (MH+); HPLC Rf: 4.67 min. (HPLC method 4); HPLC purity: 100%.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was triturated with MeOH
  3. filtrationfiltered
  4. customto provide a crude yellow solid
  5. customPurification by flash column chromatography (hexanes/ethyl acetate 5:5-1:9)