Lithium Hydroxide → 3-methyl-6,7-dihydro-5H-pyrrolo[2,1-c][1,2,4]triazole-7-carboxylic acid
反応式
[CH3:1][C:2]1[N:3]2[CH2:9][CH2:8][CH:7]([C:10]([O:12]CC)=[O:11])[C:4]2=[N:5][N:6]=1.[Li+].[OH-]>C1COCC1.O.CO>[CH3:1][C:2]1[N:3]2[CH2:9][CH2:8][CH:7]([C:10]([OH:12])=[O:11])[C:4]2=[N:5][N:6]=1参加物
4
反応条件
- 温度
- 60 °C
実験手順
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)+.