反应详情

温度

60 °C

To a solution of ethyl 6,7-dihydro-5H-pyrrolo[2,1-c][1,2,4]-triazole-7-carboxylic acid (400 mg, 2.05 mmol) in THF/water/MeOH was added LiOH (250 mg, 10.25 mmol) and the resulting solution was heated via oil bath to 60° C. for 16 h. (Round bottom was equipped with a condenser.) The solution was cooled to room temperature and concentrated to remove organic solvents. The aqueous layer was then acidified to pH of ˜5 using 2N HCl. The mixture was concentrated to dryness under vacuum, azeotroping with toluene (2×20 mL) to make sure all water was removed. The material was used without further purification with lithium chloride as a by-product. LC-MS: m/z (ES)=168 (MH)+.

1. custom(Round bottom was equipped with a condenser.) The solution
2. temperaturewas cooled to room temperature
3. concentrationconcentrated
4. customto remove organic solvents
5. concentrationThe mixture was concentrated to dryness under vacuum
6. customazeotroping with toluene (2×20 mL)
7. customwas removed
8. customThe material was used without further purification with lithium chloride as a by-product