HRID639480
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
A mixture of the title A compound, N′-(2-amino-7H-pyrrolo[2,3-d]pyrimidin-4-yl)furan-2-carbohydrazide (0.4 g, 1.55 mmol), N,O-bis(trimethylsilyl)acetamide (1.89 g, 9.3 mmol) and 2 mL of hexamethyldisilazine is heated at 120° C. overnight. After removing volatiles under vacuum, the residue is washed with 5 mL of water and the collected solid is purified by flash chromatography using EtOAc/MeOH (95/5) as eluent to give 2-(furan-2-yl)-7H-pyrrolo[3,2-e][1,2,4]triazolo[1,5-c]pyrimidin-5-amine: LC/MS (M+1=241.0). 1H NMR (DMSO-d6, 400 MHz) δ 6.57 (m, 1H), 6.70 (m, 1H), 7.01 (m, 1H), 7.18 (m, 1H), 7.36 (brs, 2H, NH2), 7.89 (s, 1H), 11.6 (br s, NH-pyrrole).
WORKUP
后处理
- customAfter removing volatiles under vacuum
- washthe residue is washed with 5 mL of water
- customthe collected solid is purified by flash chromatography