تفاعل #1747867

ord-3997275d56804cd7b800fc4a35bd29a2

معادلة التفاعل

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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحthe solution was filtered
  2. 2
    تركيزThe filtrate was concentrated
  3. 3
    workup.ADDITIONafter adding 10 ml of methanol
  4. 4
    ترشيحThe solid was filtered off with suction
  5. 5
    غسيلwashed with methanol
  6. 6
    أخرىdried at 110° C. in a vacuum
  7. 7
    أخرىdrying cabinet
  8. 8
    أخرىwere obtained

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08029919B2uspto-grants-2011_10