HRID447643

反应详情

EQUATION

反应方程式

HRID 447643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
180 °C

PROCEDURE

实验过程

4-{[(1R,3S,4S)-3-{[tert-butyl(dimethyl)silyl]oxy}-4-({[tert-butyl(dimethyl)silyl]-oxy}methyl)cyclopentyl]oxy}-6-chloro-5-fluoropyrimidine (260 mg, 0.53 mmol), (1R,2S)-2-methoxyindan-1-amine (364 mg, 2.12 mmol), and sodium carbonate (224 mg, 2.12 mmol) was weighed into a microwave reaction tube. This mixture was heated in a sealed tube under microwave irradiation at 180° C. for 2 h. The reaction mixture was diluted with DCM (100 mL), and the suspension was filtered. The filtrate was washed with saturated NH4Cl solution (100 mL), and the organic layer was dried over MgSO4. This suspension was filtered, and evaporated under vacuum. The residue was purified via silica gel column chromatography eluting with a gradient of 0 to 10% methanol in DCM to afford the title compound (313 mg, 91%).

WORKUP

后处理

  1. filtrationthe suspension was filtered
  2. washThe filtrate was washed with saturated NH4Cl solution (100 mL)
  3. dry with materialthe organic layer was dried over MgSO4
  4. filtrationThis suspension was filtered
  5. customevaporated under vacuum
  6. customThe residue was purified via silica gel column chromatography
  7. washeluting with a gradient of 0 to 10% methanol in DCM