HRID436452

反应详情

EQUATION

反应方程式

HRID 436452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-aminomethyltetrahydropyran (51 g, 0.44 mole) and ethanol (50 ml) was slowly added to a heated suspension of 6-nitroveratraldehyde (84 g, 0.4 mole) and ethanol (600 ml). The resulting solution was refluxed for 1.5 hrs and cooled overnight. The solution was concentrated to dryness and the oil was disolved in chloroform and washed with water. The chloroform extract was concentrated leaving a dark oil which crystallized upon standing. The solid was suspended in hexane and filtered (117 g. 95%), m.p. 89°-96°.

WORKUP

后处理

  1. temperatureThe resulting solution was refluxed for 1.5 hrs
  2. temperaturecooled overnight
  3. concentrationThe solution was concentrated to dryness
  4. washwashed with water
  5. extractionThe chloroform extract
  6. concentrationwas concentrated
  7. customleaving a dark oil which
  8. customcrystallized
  9. filtrationfiltered (117 g. 95%), m.p. 89°-96°