HRID1005720
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
A mixture of 2-[N-(3,4-dimethoxybenzyl)]aminothieno[3,2-d]pyrimidin-4-yl 2-thienylmethanone (0.06 g, 0.15 mmol) and TFA (2 mL) was refluxed for 2 h, cooled, concentrated in vacuo to half its original volume, diluted with CH2Cl2 (50 mL), washed with saturated sodium bicarbonate solution (3×25 mL) then brine (25 mL), dried (MgSO4), concentrated in vacuo and purified by chromatography [SiO2; heptane-EtOAc (3:1)] to give the title compound (40 mg, 100%) as a yellow solid.
WORKUP
后处理
- temperaturewas refluxed for 2 h
- temperaturecooled
- concentrationconcentrated in vacuo to half its original volume
- additiondiluted with CH2Cl2 (50 mL)
- washwashed with saturated sodium bicarbonate solution (3×25 mL)
- dry with materialbrine (25 mL), dried (MgSO4)
- concentrationconcentrated in vacuo
- custompurified by chromatography [SiO2; heptane-EtOAc (3:1)]