HRID1486572

反应详情

EQUATION

反应方程式

HRID 1486572 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 tert-butyl 5-((3-(3,5-dichlorophenylamino)-1H-1,2,4-triazol-5-ylamino)methyl)pyridin-2-ylcarbamate Compound 6 (50 mg, 111 μmol) in DCM (1 ml) was added TFA (1 ml) and the reaction was stirred for 1 hour. The reaction mixture was concentrated in vacuo and was partitioned between DCM (5 ml) and sat. NaHCO3 (3 ml). The layers were separated and the aqueous layer was extracted with DCM (3×5 ml). The combined organic solution was washed with brine (5 ml), dried over Na2SO4, filtered and concentrated to give a white solid as desired product (10.2 mg, 26% yield). MS +m/z: 350 (M+H)+

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customwas partitioned between DCM (5 ml) and sat. NaHCO3 (3 ml)
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with DCM (3×5 ml)
  5. washThe combined organic solution was washed with brine (5 ml)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated