HRID588143
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
N′-acetyl-6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridine-4-carbohydrazide (48 mg, 0.091 mmol, see synthesis of intermediate 43B) was taken up in 1,4-dioxane (1.0 ml) and Lawesson's Reagent (27.7 mg, 0.068 mmol) was added. The reaction mixture was stirred at 100° C. for 1 hr. Room temperature was attained. The reaction mixture was diluted with DCM and MeOH and was concentrated in vacuo while loading onto silica gel. The products were purified by MPLC 5-30% EtOAc/hexanes to give 2-(6-chloro-3-methoxy-1-trityl-1H-pyrazolo[4,3-c]pyridin-4-yl)-5-methyl-1,3,4-thiadiazole (44B). MS: [M+H]+ m/z 524.
WORKUP
后处理
- customRoom temperature
- concentrationwas concentrated in vacuo
- customThe products were purified by MPLC 5-30% EtOAc/hexanes