HRID2254122

反应详情

EQUATION

反应方程式

HRID 2254122 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperatureThe resulting mixture was refluxed for 3 hours
  2. customThe organic layer was recovered
  3. washwashed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customto yield a yellow oil
  8. customThis oil was purified on silica