反应详情

温度

135 °C

A stirred mixture of 2-[2-(2-ethylamino-ethylamino)-ethyl]-4-methyl-1H-pyrrole-3-carboxylic acid ethyl ester (400 mg, 1.498 mmol), lithium hydroxide monohydrate (503 mg, 11.985 mmol) in 25 ml of oxalic acid was heated to reflux at 135° C. The mixture was concentrated under reduced pressure, added with water (10 ml) and extracted with dichloromethane (20 ml×3). The combined extracts Were dried over anhydrous magnesium sulfate, filtered and concentrated wider reduced pressure to give 5-(2-ethylamino-ethyl)-3-methyl-1,5,6,7-tetrahydro-pyrrolo[3,2-c]pyridine-4-one (100 mg, 30.2%) as a brown oil.

1. temperaturewas heated
2. concentrationThe mixture was concentrated under reduced pressure
3. additionadded with water (10 ml)
4. extractionextracted with dichloromethane (20 ml×3)
5. dry with materialThe combined extracts Were dried over anhydrous magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated wider reduced pressure