HRID323627

反应详情

EQUATION

反应方程式

HRID 323627 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

6-Chloro-2-(1-naphthylamino)-2,3,4,9-tetrahydro-1H-pyrrolo[3,4-b]quinoline-1,3,9-trione (1.30 g, 3.34 mM) was stirred in methanol (0.65 L) and methanesulfonic acid (65 mL) was added. The brown suspension was heated to reflux for 16 hours during which the solids dissolved to give a brown solution. This solution was cooled to room temperature. Addition of ice (10 mL) gave a tan suspension which was stirred for 1.5 hours. The suspension was filtered (the filtrate was saved for use in Example 24) and the collected solids were washed with methanol and ether to give the title compound (0.560 g, 43%) as a dull yellow powder, mp 374-376° C.; MS(CI): 390 (M+H).

WORKUP

后处理

  1. temperatureThe brown suspension was heated
  2. temperatureto reflux for 16 hours during which the solids
  3. dissolutiondissolved
  4. customto give a brown solution
  5. customgave a tan suspension which
  6. filtrationThe suspension was filtered (the filtrate
  7. washwere washed with methanol and ether