反応 #1747868

ord-6c144124ca7c4974a84d4e5ac2edb506

反応方程式

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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

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