HRID334152

反应详情

EQUATION

反应方程式

HRID 334152 的结构方程式

PROCEDURE

实验过程

7-Bromo-2,4-dichlorothieno[3,2-d]pyrimidine (2.9 g, 10.0 mmol) was dissolved in methanol (100 mL, 2000 mmol) and added morpholine (2 mL, 22 mmol) and let the reaction mixture stir for 1.5 h. Complete reaction confirmed by LCMS. Concentrated in vacuo and diluted with water. Extracted with DCM and concentrated in vacuo again. The product was purified by silica gel chromatography (0 to 100% ethyl acetate/heptanes) on the CombiFlash® Rf system and concentrated in vacuo to give 4-(7-bromo-2-chlorothieno[3,2-d]pyrimidin-4-yl)morpholine (1.2 g, 35% yield). 1H NMR (400 MHz, CDCl3) δ 7.78 (s, 1H), 4.01 (m, 4H), 3.85 (m, 4H)

WORKUP

后处理

  1. customComplete reaction
  2. concentrationConcentrated in vacuo
  3. additiondiluted with water
  4. extractionExtracted with DCM
  5. concentrationconcentrated in vacuo again
  6. customThe product was purified by silica gel chromatography (0 to 100% ethyl acetate/heptanes) on the CombiFlash® Rf system
  7. concentrationconcentrated in vacuo