反应 #452483

ord-cbbf3a06c7d04efaab9b011975b2bcaf

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was heated
  2. 2
    温度under reflux
  3. 3
    过滤insolube matter was filtered off
  4. 4
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  5. 5
    其他to purify the same, and
  6. 6
    其他was then recrystallized from acetone

实验过程

After a mixture consisting of 7-hydroxy-3,4-dihydro-2H-1,4-benzothiazin-3-one (1.812 g, 10 mmol), 1bromo-3-chloropropane (2.362 g, 15 mmol), potassium carbate (4.146 g, 30 mmol) and acetone (40 mmol) was heated under reflux and stirring for 24 hours, insolube matter was filtered off, and the solvent was distilled off under reduced pressure. The residue was subjected to chromatography on a silica gel column (developer: chloroform) to purify the same, and was then recrystallized from acetone. The title compound (1.300 g) was obtained as yellow leaflets (yield: 50.4%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06127360uspto-grants-2000_10