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

HRID 2092686

反応式

HRID 2092686 の反応式
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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7192b305e37e41689e71164ccf5399fb
出典データセット
uspto-grants-2013_05
特許番号
US08440710B2

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