HRID580702

反应详情

EQUATION

反应方程式

HRID 580702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In 100 ml of dry tetrahydrofuran was suspended 5.00 g of 9-amino-3,4-dihydroacridin-1(2H)-one at ice temperature and 78 ml (4 eq) of 1.2M CH3Li solution in ether was added thereto at such a rate as to avoid bubbling. The reaction mixture was stirred overnight as it warmed to ambient temperature. The next day 20 ml more of the CH3Li solution was added to drive the reaction to a completion. After 0.5 hour the reaction was quenched with excess water and 4.97 g of the precipitate was collected and air dried. The product was recrystallized from MeOH/toluene. The yield was 2.06 g (38%) of granules, melting point 250° C.

WORKUP

后处理

  1. additionwas added
  2. customat such a rate as to avoid bubbling
  3. additionThe next day 20 ml more of the CH3Li solution was added
  4. customthe reaction to a completion
  5. customAfter 0.5 hour the reaction was quenched with excess water and 4.97 g of the precipitate
  6. customwas collected
  7. customair dried
  8. customThe product was recrystallized from MeOH/toluene