HRID329603

反应详情

EQUATION

反应方程式

HRID 329603 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To 2.34 g (24.1 mmol) of potassium thiocyanate in 30 ml of acetone was added 2.32 ml (20.0 mmol) of benzoyl chloride. The mixture was then refluxed for 15 min, cooled to r.t., and 3.16 g (16.3 mmol) of 2,6-diethyl-4-nitroaniline obtained from step C was added. The mixture was then refluxed for 15 min, cooled to r.t., and poured into 200 ml of ice-water. The precipitate was collected and washed with water, then dissolved in a solution comprising 0.70 g (18 mmol) of sodium hydroxide in 5 ml of water and 50 ml of ethanol. The solution was refluxed for 1 hr, cooled to r.t., poured into icewater, then the precipitate was collected, washed with water several times, and dried. The solids were then triturated with ethyl acetate to yield 2.44 g (59.2%) of product. NMR (CDCl3, d6 -DMSO):δ 1.30 (t, 6H), 2.74 (q, 4H), 6.9 (b, 2H), 7.98 (s, 2H), 9 (b, 1H).

WORKUP

后处理

  1. temperatureThe mixture was then refluxed for 15 min
  2. temperatureThe mixture was then refluxed for 15 min
  3. temperaturecooled to r.t.
  4. customThe precipitate was collected
  5. washwashed with water
  6. temperatureThe solution was refluxed for 1 hr
  7. temperaturecooled to r.t.
  8. additionpoured into icewater
  9. customthe precipitate was collected
  10. washwashed with water several times
  11. customdried
  12. customThe solids were then triturated with ethyl acetate