HRID19511

反应详情

EQUATION

反应方程式

HRID 19511 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 2.18 g (11.55 mmol) of 3-tert-Butoxycarbonylamino-propionic acid in 20 ml of DMF were added 3.78 g (11.55 mmol) TOTU. After 15 min at room temperature 2.0 g (11.55 mmol) of 2-methyl-quinoline-4,6-diamine and 2.66 g (23 mmol) of N-ethylmorpholine were added. After 24 h stirring at room temperature the solution was evaporated and the residue was treated with a saturated aqueous solution of NaHCO3. The aqueous solution was extracted with ethyl acetate. The separated organic layer was dried (Na2SO4) and evaporated. The residue was treated with 20 ml 90% trifluoroacetic acid for 2 h. After evaporation the residue was dissolve in water and extracted with ethyl acetate. The aqueous layer was lyophilized to yield 5.15 g (76%) of the title compound. MS 245.1 (M+1)+.

WORKUP

后处理

  1. customwas evaporated
  2. additionthe residue was treated with a saturated aqueous solution of NaHCO3
  3. extractionThe aqueous solution was extracted with ethyl acetate
  4. dry with materialThe separated organic layer was dried (Na2SO4)
  5. customevaporated
  6. additionThe residue was treated with 20 ml 90% trifluoroacetic acid for 2 h
  7. customAfter evaporation the residue
  8. dissolutionwas dissolve in water
  9. extractionextracted with ethyl acetate