Potassium Carbonate → 3,4-Bis(2,2,2-trifluoroethoxy)nitrobenzene

HRID 2412332노트

반응식

HRID 2412332 반응식
[C:1](=[O:4])([O-])[O-].[K+].[K+].FC(F)(F)S([O:12][CH2:13][C:14]([F:17])([F:16])[F:15])(=O)=O.[N+:20]([C:23]1[CH:24]=[C:25](O)[C:26](=[CH:28][CH:29]=1)O)([O-:22])=[O:21]>CC(C)=O>[F:17][C:14]([F:15])([F:16])[CH2:13][O:12][C:28]1[CH:29]=[C:23]([N+:20]([O-:22])=[O:21])[CH:24]=[CH:25][C:26]=1[O:4][CH2:1][C:14]([F:17])([F:16])[F:15]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 803662,2,2-Trifluoroethyl trifluoromethanesulfonateHCID 35051094-Nitrocatechol

생성물 1

HCID 133704333,4-Bis(2,2,2-trifluoroethoxy)nitrobenzene

시약·촉매·용매 1

HCID 180Acetone용매2회

실험 절차

To a refluxing mixture of 12.7 g (0.092 mole) of potassium carbonate, 21.3 g. (0.092 mole) of 2,2,2-trifluoroethyl trifluoromethanesulfonate and 62 ml. of acetone is added dropwise 6.2 g. (0.040 mole) of 4-nitrocatechol in 62 ml. of acetone over about 2.5 hours. Refluxing is continued for a total of 24 hours, then the solution is evaporated. The residue is mixed with equal volumes of water and diethyl ether. The ether layer is separated, washed with water and saturated sodium chloride solution and dried. Evaporation provides crude 3,4-bis(2,2,2-trifluoroethoxy)nitrobenzene. Chromatographic purification on a silica gel column is effected by eluting with mixtures of chloroform and hexane. Recrystallization from cyclohexane with a small amount of benzene provides solid product, m.p. 63°-65° C.

후처리

  1. temperatureRefluxing
  2. customis continued for a total of 24 hours
  3. customthe solution is evaporated
  4. additionThe residue is mixed with equal volumes of water and diethyl ether
  5. customThe ether layer is separated
  6. washwashed with water and saturated sodium chloride solution
  7. customdried
  8. customEvaporation

출처 및 근거

ORD 기록
ord-a2c1c22ccc03492188752860682324a1
출처 데이터셋
uspto-grants-1985_01
특허 번호
US04491584

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