Hydrochloric Acid → 2-(3-Fluoro-4-methylphenyl)benzonitrile

HRID 234758

反応式

HRID 234758 の反応式
CC1(C)O[C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=2[C:13]2[CH:18]=[CH:17][C:16]([CH3:19])=[C:15]([F:20])[CH:14]=2)=[N:4]C1.N1C=CC=CC=1.P(Cl)(Cl)(Cl)=O.Cl>CCOCC>[F:20][C:15]1[CH:14]=[C:13]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:5]#[N:4])[CH:18]=[CH:17][C:16]=1[CH3:19]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 24813Phosphorus oxychlorideHCID 545155994,5-Dihydro-5,5-dimethyl-2-(3'-fluoro-4'-methyl-biphenyl-2-yl)oxazole

生成物 1

HCID 542386242-(3-Fluoro-4-methylphenyl)benzonitrile

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

97.0 g (343 mmol) of the compound from Example III are initially introduced into 500 ml of pyridine, and 31.3 ml (343 mmol) of phosphorus oxychloride are added at 0° C., while stirring. The mixture is heated slowly, and is finally boiled under reflux for 1 hour. After cooling to room temperature, ether and an amount of 1M hydrochloric acid such that the pH of the aqueous phase is 1.5 are added. The organic phase is washed three more times with 1M sulphuric acid, dried with sodium sulphate and evaporated on a rotary evaporator and the residue is freed from the residual solvent under a high vacuum.

後処理

  1. additionare added at 0° C.
  2. temperatureThe mixture is heated slowly
  3. temperatureunder reflux for 1 hour
  4. additionare added
  5. washThe organic phase is washed three more times with 1M sulphuric acid
  6. dry with materialdried with sodium sulphate
  7. customevaporated on a rotary evaporator

出典と根拠

ORDレコード
ord-03a275f73cc44f37bf751a999adad78a
出典データセット
uspto-grants-1997_01
特許番号
US05596006

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