反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a mixture of 4.5 mL of phosphorus oxychloride and 20 drops of dimethylaniline in 50 mL of toluene was added 4.2 g of 5,6,7,8-tetrahydro-2-methyl-4-quinazolone. The resulting mixture was refluxed for 3 hours and then cooled to room temperature. The reaction mixture was poured into a ice cold aqueous potassium carbonate. After stirring for 5 minutes the mixture was added to diethyl ether/water. The organic layer was recovered washed with brine, dried over anhydrous magnesium sulfate, filtered and evaporated to yield a yellow oil. This oil was purified on silica to yield the desired compound as a light yellow solid (4.45 g, 95%): 1H NMR (DMSO-d6, 300 MHz) δ 2.78 (m, 2H), 2.64 (m, 2H), 2.50 (s, 3H), 1.78 (m, 4H).
WORKUP
后处理
- temperatureThe resulting mixture was refluxed for 3 hours
- customThe organic layer was recovered
- washwashed with brine
- dry with materialdried over anhydrous magnesium sulfate
- filtrationfiltered
- customevaporated
- customto yield a yellow oil
- customThis oil was purified on silica