反应 #8196

反应方程式

{2-[7-(3-Cyano-pyridin-2-yloxy)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester

1,4 dioxane

hydrochloric acid

1,4 dioxane

→

amine

收率 83.0%

Amine 12

收率 83.0%

反应条件

后处理

1. 1
   温度The mixture is cooled to zero degrees Celsius in an ice/water bath
2. 2
   其他The solvent is evaporated
3. 3
   萃取is extracted three times with 50 mL of ethyl acetate
4. 4
   干燥dried with sodium sulfate
5. 5
   过滤filtered
6. 6
   其他the solvent removed in vacuo

实验过程

{2-[7-(3-Cyano-pyridin-2-yloxy)-1H-indol-3-yl]-1,1-dimethyl-ethyl}-carbamic acid tert-butyl ester (119 mg, 0.293 mmol) is dissolved in 10 mL of 1,4 dioxane. The mixture is cooled to zero degrees Celsius in an ice/water bath. To the mixture is added 10 mL of 4N hydrochloric acid in 1,4 dioxane, and the resulting mixture is stirred at zero degrees, under nitrogen, for five hours. The solvent is evaporated, and the residue is taken up in water. The pH of the water is adjusted to 9 using sodium bicarbonate, and is extracted three times with 50 mL of ethyl acetate. The organic layers are combined, dried with sodium sulfate, filtered, and the solvent removed in vacuo to give 218 mg of the title amine (83%). FDMS m/e=307 (M++1).

来源