反应 #1747868

ord-6c144124ca7c4974a84d4e5ac2edb506

反应方程式

CCN(CC)CC
triethylamine
O=C(Cl)c1ccccc1
benzoyl chloride
O=S1(=O)c2ccccc2N(c2ccc(O)cc2)c2ccccc21
10-(4-hydroxyphenyl)phenothiazine 5,5-dioxide
O=C(Oc1ccc(N2c3ccccc3S(=O)(=O)c3ccccc32)cc1)c1ccccc1
4-(5,5-Dioxophenothiazin-10-yl)phenyl benzoate

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISTILLATIONthe solvent was distilled off
  2. 2
    workup.STIRRINGstirred at 75° C. for 30 min
  3. 3
    过滤The solid was filtered off with suction while hot,
  4. 4
    洗涤washed with hot water
  5. 5
    其他dried at 120° C. in a forced-air drying cabinet
  6. 6
    其他were obtained

实验过程

0.68 g (6.68 mmol) of triethylamine and 0.34 g (2.44 mmol) of benzoyl chloride were added to a solution of 0.72 g (2.22 mmol) of 10-(4-hydroxyphenyl)phenothiazine 5,5-dioxide in 120 ml of acetonitrile. After stirring at room temperature for 45 min, the solvent was distilled off. The residue was taken up in 100 ml of hot water and stirred at 75° C. for 30 min. The solid was filtered off with suction while hot, washed with hot water and dried at 120° C. in a forced-air drying cabinet. 0.87 g (92% of theory) of colorless microcrystals having an m.p. of 233-235° C. were obtained.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08029919B2uspto-grants-2011_10