Water → 1-(4-Bromophenyl)-2-phenylethane-1,2-dione

HRID 1595947노트

반응식

HRID 1595947 반응식
Cl(O)(=O)(=O)=O.[OH2:6].O.O.O.[N+]([O-])([O-])=O.[Tl+3].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[Br:23][C:24]1[CH:29]=[CH:28][C:27]([C:30]([CH2:32][C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)=[O:31])=[CH:26][CH:25]=1>C(Cl)Cl.COCCOC>[Br:23][C:24]1[CH:25]=[CH:26][C:27]([C:30]([C:32]([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)=[O:6])=[O:31])=[CH:28][CH:29]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 24247Perchloric AcidHCID 5197381-(4-Bromophenyl)-2-phenylethanoneHCID 11270721Nitric acid,thallium(3+) salt, trihydrate (9CI)

생성물 1

HCID 2367011-(4-Bromophenyl)-2-phenylethane-1,2-dione

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 80711,2-Dimethoxyethane용매

실험 절차

Perchloric acid (250 mL), water (250 mL), ethylene glycol dimethyl ether (glyme) (500 mL), thallium (III) nitrate trihydrate (222.0 g, 0.5 mol) and 4-bromodeoxybenzoin (68.75 g, 0.25 mol) are charged to a 2-liter round bottom 3-necked flask equipped with a reflux condenser and a mechanical stirrer. The reaction mixture is heated under nitrogen to reflux for 6 hours. After cooling to ambient temperature, methylene chloride (500 mL) is added. The resulting bilayer is decanted off the precipitated Tl(I) salts formed. The layers are separated and the organic layer is washed with water, saturated aqueous NaHCO3 and brine, followed by recrystallization of the resulting solid from 2-propanol gives the title compound.

후처리

  1. customequipped with a reflux condenser and a mechanical stirrer
  2. temperatureThe reaction mixture is heated under nitrogen
  3. temperatureto reflux for 6 hours
  4. customThe resulting bilayer is decanted off the precipitated Tl(I) salts
  5. customformed
  6. customThe layers are separated
  7. washthe organic layer is washed with water, saturated aqueous NaHCO3 and brine
  8. customfollowed by recrystallization of the resulting solid from 2-propanol

출처 및 근거

ORD 기록
ord-af2beb105d0046fb8351b674e61a5cf8
출처 데이터셋
uspto-grants-2001_09
특허 번호
US06288188B1

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