HRID2219579

反应详情

EQUATION

反应方程式

HRID 2219579 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 40 mg (0.088 mmol) of 6-Methyl-3-(pyrimidin-5-ylamino)-pyridine-2-carboxylic acid [4-(tert-butyl-dimethyl-silanyloxymethyl)-thiazol-2-yl]-amide in 1 ml of methylene chloride was added 200 mg (1.75 mmol, 20.0 equiv.) of Trifluoroacetic acid. After stirring for 2 h at room temperature, saturated sodium carbonate solution was added, and the pH was adjusted to 8. The aqueous phase was extracted three times with methylene chloride. The combined organic phases were dried over magnesium sulfate, filtered and concentrated in vaccuo. The residue (28 mg, yellow solid) was triturated with Diisopropyl ether, filtered and dried to yield the title compound (17 mg, 57%) as a light yellow solid, MS (ISP): m/e=343.1 (M+H+).

WORKUP

后处理

  1. extractionThe aqueous phase was extracted three times with methylene chloride
  2. dry with materialThe combined organic phases were dried over magnesium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated in vaccuo
  5. customThe residue (28 mg, yellow solid) was triturated with Diisopropyl ether
  6. filtrationfiltered
  7. customdried