Hydrochloric Acid → Nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene

HRID 2092686노트

반응식

HRID 2092686 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][CH:3]=1.[F:11][C:12]([F:17])([F:16])[CH:13]([OH:15])[CH3:14].C(=O)([O-])[O-].[Cs+].[Cs+].Cl>CC#N.O.C(OCC)(=O)C>[N+:8]([C:5]1[CH:6]=[CH:7][C:2]([O:15][CH:13]([CH3:14])[C:12]([F:17])([F:16])[F:11])=[CH:3][CH:4]=1)([O-:10])=[O:9]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 9590p-FluoronitrobenzeneHCID 97741,1,1-Trifluoro-2-propanolHCID 10796Cesium carbonate

생성물 1

HCID 66577895Nitro-4-(2,2,2-trifluoro-1-methyl-ethoxy)-benzene

시약·촉매·용매 3

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1-fluoro-4-nitrobenzene (4.24 g, CAS Reg. No. 350-46-9), 1,1,1-trifluoro-propan-2-ol (4.56 g, CAS Reg. No. 374-01-6) and cesium carbonate (13.04 g) in CH3CN (50 mL) was heated to reflux for 10 hours. Then, the reaction mixture was cooled, acidified with conc. HCl and then distributed between ethyl acetate and water. The organic layer was separated, washed with brine and evaporated to provide the title compound (6.74 g) that was used without further purification. Rf: 0.38 (silica gel, ether/heptane 1:4).

후처리

  1. temperatureto reflux for 10 hours
  2. temperatureThen, the reaction mixture was cooled
  3. customThe organic layer was separated
  4. washwashed with brine
  5. customevaporated

출처 및 근거

ORD 기록
ord-7192b305e37e41689e71164ccf5399fb
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08440710B2

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