HRID522886

反应详情

EQUATION

反应方程式

HRID 522886 的结构方程式

CONDITIONS

反应条件

温度
95 °C

PROCEDURE

实验过程

To a vial charged with 6-bromo-2-(4-chloro-1,3,5-triazin-2-yl)-1,2,3,4-tetrahydroisoquinoline (163 mg, 499 μmol) and 3-amino-2-methylbenzamide (75 mg, 499 μmol) was added N-ethyl-N-isopropylpropan-2-amine (174 μl, 999 μmol) and propan-2-ol (1665 μl, 499 μmol). The vial was sealed and heated to 95° C. overnight. The product was purified by reverse phase liquid chromatography using TFA as a modifier. Fractions containing the product were combined and neutralized with saturated NaHCO3 (35 mL). The product was extracted with DCM (3×30 mL). The organics were separated, dried over Na2SO4, and filtered to afford 3-(4-(6-bromo-3,4-dihydroisoquinolin-2(1H)-yl)-1,3,5-triazin-2-ylamino)-2-methylbenzamide (55 mg, 25%) as a white solid upon drying.

WORKUP

后处理

  1. customThe vial was sealed
  2. customThe product was purified by reverse phase liquid chromatography
  3. additionFractions containing the product
  4. extractionThe product was extracted with DCM (3×30 mL)
  5. customThe organics were separated
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered