HRID495471

反应详情

EQUATION

反应方程式

HRID 495471 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of N-tert-butyloxycarbonyl-6-methoxy-3-aminoquinoline (Step F, 3 g, 0.011 mol) in CH2Cl2 (50 mL) cooled at 0° C. was added TFA (8.4 mL, 0.11 mL). The reaction mixture was warmed to RT and stirred for 8 h. The reaction mixture was concentrated under vacuum. The residue was suspended into MTBE. The yellow solid was filtered off and washed with MTBE. The dry yellow solid was suspended in NaOH 1N and the suspension was stirred for 15 min. The resulting slurry was filtered. The solid was washed with water and dried over P2O5 to give 6-methoxy-3-aminoquinoline as a white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under vacuum
  2. filtrationThe yellow solid was filtered off
  3. washwashed with MTBE
  4. stirringthe suspension was stirred for 15 min
  5. filtrationThe resulting slurry was filtered
  6. washThe solid was washed with water
  7. dry with materialdried over P2O5