HRID1241374
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
- 75 °C
PROCEDURE
实验过程
Crude N-(1-{6-[(5-cyano-1,3-thiazol-2-yl)amino]pyrimidin-4-yl}piperidin-3-yl)-2,2,2-trifluoroacetamide 9-5 (0.9 mmol) was suspended/dissolved in methanol/dimethoxyether (5 mL/2 mL) and potassium carbonate (1.8 mmol). This was warmed to 75° C. and stirred overnight. The product was purified on a preparative hplc and isolated via lyophilization from dioxane/water to produce 9-6. Hi-Res MS: calc: 302.1183 found: 302.1190. 1NMR(CD3OD): 8.31 ppm (s, 1H); 7.87 ppm (s, 1H); 6.09 ppm (s, 1H); 4.21 ppm (d, 1H); 4.07 ppm (d, 1H); 3.60 ppm (m, 1H); 2.95 ppm (m, 1H); 2.75 ppm (m, 1H); 2.00 ppm (m, 1H); 1.77 ppm (m, 1H); 1.54 ppm (m, 1H); 1.37 ppm (m, 1H).
WORKUP
后处理
- customThe product was purified on a preparative hplc and
- customisolated via lyophilization from dioxane/water
- customto produce 9-6