Hydrochloric Acid → 4-Bromo-2,6-dimethylphenyl trifluoromethanesulfonate

HRID 2220623ノート

反応式

HRID 2220623 の反応式
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].[Br:16][C:17]1[CH:22]=[C:21]([CH3:23])[C:20](O)=[C:19]([CH3:25])[CH:18]=1.N1C=CC=CC=1.Cl>C(Cl)Cl.C(OCC)(=O)C>[F:1][C:2]([F:15])([F:14])[S:3]([O:6][C:20]1[C:21]([CH3:23])=[CH:22][C:17]([Br:16])=[CH:18][C:19]=1[CH3:25])(=[O:5])=[O:4]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 169194-Bromo-2,6-dimethylphenolHCID 67749Trifluoromethanesulfonic anhydride

生成物 1

HCID 231343334-Bromo-2,6-dimethylphenyl trifluoromethanesulfonate

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Trifluoromethanesulfonic anhydride (1.004 mL) was added to an ice-cooled mixture of 4-bromo-2,6-dimethylphenol (1.00 g) and pyridine (0.482 mL) in methylene chloride (5 mL) with stirring. After being stirred for 10 minutes, the reaction mixture was poured into a mixture of 1 mol/L hydrochloric acid and ethyl acetate. The organic layer was separated, washed with water and brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: diethyl ether/n-hexane=1/20) to afford 4-bromo-2,6-dimethylphenyl trifluoromethanesulfonate (1.439 g).

後処理

  1. temperaturecooled
  2. stirringAfter being stirred for 10 minutes
  3. customThe organic layer was separated
  4. washwashed with water and brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (eluent: diethyl ether/n-hexane=1/20)

出典と根拠

ORDレコード
ord-31181d6510d442a09db40694d9f917d6
出典データセット
uspto-grants-2008_08
特許番号
US07417169B2

反応ノート

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