반응 #1747868

ord-6c144124ca7c4974a84d4e5ac2edb506

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.DISTILLATIONthe solvent was distilled off
  2. 2
    workup.STIRRINGstirred at 75° C. for 30 min
  3. 3
    여과The solid was filtered off with suction while hot,
  4. 4
    세척washed with hot water
  5. 5
    기타dried at 120° C. in a forced-air drying cabinet
  6. 6
    기타were obtained

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08029919B2uspto-grants-2011_10