Реакция #1747868

ord-6c144124ca7c4974a84d4e5ac2edb506

Уравнение реакции

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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08029919B2uspto-grants-2011_10