HRID1072069
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
- 100 °C
PROCEDURE
实验过程
A suspension of of 5-methyl-3H-pyrrolo[2,1-f][1,2,4]triazin-4-one (2.57 gm, 17.2 mmole) in POCl3 (28 mL) was heated at 100° C. for 40 min. The excess reagent was removed under vacuum and the residue was dissolved in DCM (300 mL). This was washed with water, dried (Na2SO4), and the solvent removed. Flash chromatography on silica gel using DCM as eluent afforded the product as a yellow solid (2.38 gm, 82%). 1HNMR (CDCl3): δ 2.63 (s, 3H), 6.74 (d, 1H, J=2 Hz), 7.74 (d, 1H, J=2 Hz), 8.05 (s, 1H).
WORKUP
后处理
- customThe excess reagent was removed under vacuum
- dissolutionthe residue was dissolved in DCM (300 mL)
- washThis was washed with water
- dry with materialdried (Na2SO4)
- customthe solvent removed