反应详情

A solution of 2-ethoxycarbonylmethyl-4-(2-morpholin-4-yl-ethoxy)-benzoic acid (2.65 g, 10.0 mmole) and saturated ammonia in dioxane (15 mL) in a pressure bottle is stirred and heated using an oil bath at 95° C. overnight. This mixture is cooled and followed by Ic/ms, reaction not complete. The dioxane is evaporated and replaced with 15 mL of 7M ammonia in methanol and heated overnight in a pressure bottle using an oil bath at 70° C., still a small amount of starting material left. The solvent is removed in vacuo and used as is in the next step MS (ESI): m/z 309.3 (M+H).

1. temperatureheated
2. customat 95° C.
3. customovernight
4. temperatureThis mixture is cooled
5. customfollowed by Ic/ms, reaction not complete
6. customThe dioxane is evaporated
7. temperatureheated overnight in a pressure bottle
8. customat 70° C.
9. waitstill a small amount of starting material left
10. customThe solvent is removed in vacuo