Ammonium Chloride → 4-(4-n-Propylphenyl)trifluorotoluene

HRID 486343

반응식

HRID 486343 반응식
[CH2:1]([C:4]1[CH:9]=[CH:8][C:7](Br)=[CH:6][CH:5]=1)[CH2:2][CH3:3].[Mg].Br[C:13]1[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][CH:14]=1.[Cl-].[NH4+]>C1COCC1.[Br-].[Zn+2].[Br-]>[CH2:1]([C:4]1[CH:9]=[CH:8][C:7]([C:13]2[CH:18]=[CH:17][C:16]([C:19]([F:22])([F:21])[F:20])=[CH:15][CH:14]=2)=[CH:6][CH:5]=1)[CH2:2][CH3:3]

참가 물질

7

반응물 4

HCID 25517Ammonium ChlorideHCID 67872Benzene, 1-bromo-4-(trifluoromethyl)-HCID 1363741-Bromo-4-propylbenzeneHCID 5462224Magnesium

생성물 1

HCID 149851934-(4-n-Propylphenyl)trifluorotoluene

시약·촉매·용매 2

HCID 10421208Zinc bromide촉매HCID 8028Tetrahydrofuran용매3회

실험 절차

11.2 g of anhydrous zinc bromide in 25 ml of THF are added dropwise at about 0° to a Grignard solution prepared from 20 g of 4-n-propylbromobenzene and 2.4 g of magnesium turnings in 100 ml of THF. After the mixture has been stirred for 2 hours, a mixture of 22.5 g of 4-bromotrifluorotoluene, 1.5 g of [(diphenylphosphine)ferrocenyl]palladium(II) chloride and 25 ml of THF is added dropwise, and the mixture is stirred for 24 hours at room temperature and poured into 100 ml of saturated ammonium chloride solution. Customary work-up gives 4-(4-n-propylphenyl)trifluorotoluene, M.p. 97° C., Δε=14.2, viscosity η (20° C.)=6 mm2 /s.

후처리

  1. additionis added dropwise
  2. stirringthe mixture is stirred for 24 hours at room temperature

출처 및 근거

ORD 기록
ord-9a287455070b4912bc1db937bf0676e8
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292454

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