反应详情

温度

60 °C

To a solution of ethyl 3-methyl-6,7-dihydro-5H-pyrrolo[2,1-c][1,2,4]-triazole-7-carboxylate (400 mg, 2.05 mmol) from step A in THF/water/MeOH was added LiOH (250 mg, 10.3 mmol) and the resulting solution was heated to 60° C. for 16 h. 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. temperatureThe solution was cooled to room temperature
2. concentrationconcentrated
3. customto remove organic solvents
4. concentrationThe mixture was concentrated to dryness under vacuum
5. customazeotroping with toluene (2×20 mL)
6. customwas removed
7. customThe material was used without further purification with lithium chloride as a by-product