Acetic Acid → 2-(4-Carboxyphenyl)-2-phenylhexafluoropropane

HRID 1975861

반응식

HRID 1975861 반응식
C[C:2]1[CH:7]=[CH:6][C:5]([C:8]([C:17]2[CH:22]=[CH:21]C=[CH:19][CH:18]=2)([C:13]([F:16])([F:15])[F:14])[C:9]([F:12])([F:11])[F:10])=[CH:4][CH:3]=1.Br.[C:24]([OH:27])(=[O:26])[CH3:25]>O.O.O.O.C([O-])(=O)C.[Co+2].C([O-])(=O)C.O.O.O.O.C([O-])(=O)C.[Mn+4].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C>[C:24]([C:25]1[CH:21]=[CH:22][C:17]([C:8]([C:5]2[CH:4]=[CH:3][CH:2]=[CH:7][CH:6]=2)([C:13]([F:14])([F:15])[F:16])[C:9]([F:11])([F:12])[F:10])=[CH:18][CH:19]=1)([OH:27])=[O:26]

참가 물질

6

반응물 3

HCID 176Acetic AcidHCID 260Hydrogen Bromide2회HCID 147667062-(4-Methylphenyl)-2-phenylhexafluoropropane

생성물 1

HCID 147667072-(4-Carboxyphenyl)-2-phenylhexafluoropropane

시약·촉매·용매 2

HCID 61372Cobalt(II) acetate tetrahydrate촉매HCID 178476541HCID 178476541, 화합물촉매

반응 조건

온도
180 °C

실험 절차

298 g of 2-(4-methylphenyl)-2-phenylhexafluoropropane, 2.49 g of cobalt(II) acetate tetrahydrate, 2.45 g of manganese(IV) acetate tetrahydrate and 0.41 g of hydrogen bromide (corresponding to 4.1 g of a 10% strength HBr solution in glacial acetic acid) were initially introduced into a 1 l glass autoclave. The mixture was heated to about 180° C. under an oxygen pressure of 6.5 bar and under an exothermic reaction and was left at 170°-180° C. for 1 hour. The reaction solution was cooled to about 100° C. and 200 g of acetic acid were then distilled off. 275 g of water were slowly added to the solution remaining in the flask (about 600 g) at the boiling point. The carboxylic acid which had crystallized out was filtered off with suction, washed twice with 75 ml of 50% strength aqueous acetic acid each time and five times with 85 ml of water each time and dried at 60° C./60 mbar. Yield: 311 g (95.5% of theory) melting point: 153°-155° C., small colorless crystals.

후처리

  1. customunder an exothermic reaction
  2. temperatureThe reaction solution was cooled to about 100° C.
  3. distillation200 g of acetic acid were then distilled off
  4. addition275 g of water were slowly added to the solution
  5. customThe carboxylic acid which had crystallized out
  6. filtrationwas filtered off with suction
  7. washwashed twice with 75 ml of 50% strength aqueous acetic acid each time and five times with 85 ml of water each time
  8. customdried at 60° C./60 mbar

출처 및 근거

ORD 기록
ord-1df8b80c3bce4765a3456ac59f467e1b
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05288908

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