HRID238225

反应详情

EQUATION

反应方程式

HRID 238225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

In a test tube containing of 4-Chloro-2-{1-[4-(4-methoxy-benzenesulfonyl)-piperazin-1-yl]-ethyl}-quinazoline (38.0 mg, 0.089 mmol) in THF (2 ml) was added MeOH (280.0 mg, 8.9 mmol). The reaction was heated at 60° C. for 0.5 hour. The solution was concentrated under reduced pressure. The residue was partitioned between water (2 ml) and dichloromethane (5 ml). The organic layer was dried over magnesium sulfate, filtered and concentrated under reduced pressure. The solvent was removed under vacuum. The resulting residue was re-dissolvent in MeOH (2 ml) and purified by HPLC (Gilson-215, 0.035% TFA in acetonitrile and 0.05% water as mobile phase). The product was collected and dried under reduced pressure to give 4-Methoxy-2-{1-[4-(4-methoxy-benzenesulfonyl)-piperazin-1-yl]-ethyl}-quinazoline (Yield 4.43 mg, 11.13%). MS m/z calc. 442.17, found (ESI); 443.4 (M+1)+. Retention time 2.40 minutes.

WORKUP

后处理

  1. concentrationThe solution was concentrated under reduced pressure
  2. customThe residue was partitioned between water (2 ml) and dichloromethane (5 ml)
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe solvent was removed under vacuum
  7. dissolutionThe resulting residue was re-dissolvent in MeOH (2 ml)
  8. custompurified by HPLC (Gilson-215, 0.035% TFA in acetonitrile and 0.05% water as mobile phase)
  9. customThe product was collected
  10. customdried under reduced pressure