Реакция #1747867

ord-3997275d56804cd7b800fc4a35bd29a2

Уравнение реакции

O=S1(=O)c2ccccc2N(c2ccc(OCc3ccccc3)cc2)c2ccccc21
10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide
O=C[O-].[NH4+]
ammonium formate
O=S1(=O)c2ccccc2N(c2ccc(O)cc2)c2ccccc21
10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Фильтрацияthe solution was filtered
  2. 2
    КонцентрированиеThe filtrate was concentrated
  3. 3
    workup.ADDITIONafter adding 10 ml of methanol
  4. 4
    ФильтрацияThe solid was filtered off with suction
  5. 5
    Промывкаwashed with methanol
  6. 6
    Другоеdried at 110° C. in a vacuum
  7. 7
    Другоеdrying cabinet
  8. 8
    Другоеwere obtained

Методика

3.10 g (7.50 mmol) of 10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide, 2.30 g (35.7 mmol) of 98% ammonium formate and 7.5 g of 10% palladium on activated carbon were heated to boiling under reflux in 225 ml of acetone for 1 hour. After cooling to room temperature, the solution was filtered. The filtrate was concentrated and, after adding 10 ml of methanol, stirred overnight. The solid was filtered off with suction, washed with methanol and dried at 110° C. in a vacuum drying cabinet. 1.47 g (61% of theory) of analytically pure light gray microcrystals having an m.p. of 308-311° C. were obtained.

Источник

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