反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- 90 °C
PROCEDURE
实验过程
A mixture of 2-chloro-7-methoxy-8-(2-propyl)quinazoline (200 mg, 0.76 mmol) and aniline (212 mg, 2.28 mmol) in acetonitrile (3 mL) was heated at 90° C. for 60 hours in a sealed tube. The solvent was removed under reduced pressure, to the residue 5% sodium carbonate solution was added. The product was extracted with ethyl acetate (3×40 mL). The combined organic extract was washed with brine, dried (Na2SO4), and concentrated. The product was purified on a column of silica gel to give the title compound as a yellow solid (90 mg, 37%), mp 187–188° C.; 1H NMR (CDCl3) δ: 1.72–2.30 (complex, 8H, 4×CH2), 3.96 (s, 3H, OCH3), 4.33 (m, 1H, CH), 7.23–7.41 (m, 2H, Ar-H), 7.58 (d, 1H, Ar-H), 7.83 (d, 2H, Ar-H), 8.93 (s, 1H, Ar-H); MS: m/z 319.81, C20H21N3O; Analysis: Calcd.: C, 75.21; H, 6.63; N, 13.16. Found: C, 75.03; H, 6.73; N, 13.05.
WORKUP
后处理
- customThe solvent was removed under reduced pressure, to the residue 5% sodium carbonate solution
- additionwas added
- extractionThe product was extracted with ethyl acetate (3×40 mL)
- extractionThe combined organic extract
- washwas washed with brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customThe product was purified on a column of silica gel