反应详情
EQUATION
反应方程式
REACTANTS
反应物
Pyridine
C5H5N
未命名化合物
6-Amino-4-chloro-1-phenol-2-sulfonic acid
C6H6ClNO4S
3H-1,2,3-Triazolo[4,5-b]pyridine, 3-hydroxy-
C5H4N4O
Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)
C10H15F6N6OP
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
After 92 mg (0.33 mmol) of the compound obtained in Step 1, 130 mg (0.33 mmol) of HATU, 45 mg (0.33 mmol) of HOAt and 77 mg (0.33 mmol) of 3-amino-5-chloro2-hydroxybenzenesulfonic acid were suspended in 1.0 ml of DMF, 0.25 ml of pyridine was added to the suspension. The mixture was stirred at room temperature overnight. The solvent was removed by distillation and the mixture was purified in accordance with the purification step A to give the intermediate. The crude product was dissolved in 4.0 ml of TFA. The solution was stirred at room temperature for an hour. The solvent was removed by distillation and the mixture was purified in accordance with the purification step A to give 47.2 mg of the title compound.
WORKUP
后处理
- customThe solvent was removed by distillation
- customthe mixture was purified in accordance with the purification step A
- customto give the intermediate
- stirringThe solution was stirred at room temperature for an hour
- customThe solvent was removed by distillation
- customthe mixture was purified in accordance with the purification step A