反应详情

温度

0 °C

Ethyl 3-(1-trityl-1H-imidazol-4-yl)-1H-pyrazole-5-carboxylate (4.01 mmol, 1.8 g) was dissolved in ethanol (20 ml) and cooled to 0° C. NaOH 2 M solution (8.03 mmol, 4.01 ml) was added and the mixture was stirred at RT for an hour. The mixture was heated to 60° C. and stirred for 10 h. Ethanol was evaporated and the residue was diluted with water. The pH was adjusted to 4 with 1 M HCl solution which precipitated the product. The precipitate was removed by filtration and washed with water. The solid was dried under vacuum. 1.5 g of the title compound was obtained. 1H-NMR (400 MHz, DMSO-d6): δ 6.75 (bs, 1H), 7.08-7.17 (m, 6H), 7.18-7.34 (m, 5H), 7.36-7.49 (m, 8H). LC-MS: [M−1]=419.1.

1. temperatureThe mixture was heated to 60° C.
2. stirringstirred for 10 h
3. customEthanol was evaporated
4. additionthe residue was diluted with water
5. customprecipitated the product
6. customThe precipitate was removed by filtration
7. washwashed with water
8. customThe solid was dried under vacuum