반응 #1747867

ord-3997275d56804cd7b800fc4a35bd29a2

반응 방정식

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

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the solution was filtered
  2. 2
    농축The filtrate was concentrated
  3. 3
    workup.ADDITIONafter adding 10 ml of methanol
  4. 4
    여과The solid was filtered off with suction
  5. 5
    세척washed with methanol
  6. 6
    기타dried at 110° C. in a vacuum
  7. 7
    기타drying cabinet
  8. 8
    기타were obtained

실험 절차

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.

출처

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