Hydrochloric Acid → (+)-4-(3'-Methylpentanoyl)biphenyl

HRID 26336

반응식

HRID 26336 반응식
[C:1]1([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Cl-].[Cl-].[Al+3].[CH3:17][CH:18]([CH2:23][CH3:24])[CH2:19][C:20](Cl)=[O:21].Cl>[N+](C1C=CC=CC=1)([O-])=O.O>[CH3:17][CH:18]([CH2:23][CH3:24])[CH2:19][C:20]([C:4]1[CH:5]=[CH:6][C:1]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[CH:2][CH:3]=1)=[O:21]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 7095BiphenylHCID 6451240Aluminum(III) ChlorideHCID 126482793-Methylpentanoyl chloride

생성물 1

HCID 21322796(+)-4-(3'-Methylpentanoyl)biphenyl

시약·촉매·용매 2

HCID 962Water용매HCID 7416Nitrobenzene용매

반응 조건

온도
-7 °C

실험 절차

To commercially available biphenyl (0.08 mole) and anhydrous aluminium trichloride (0.1 mole) dissolved in dry nitrobenzene (90ml), (+)-3-methylpentanoylchloride (0.1mole) the preparation of which is known and described in United Kingdom Patent Application No. 36211/75), is added in drops, the temperature being maintained at about -7° C. during the addition. The mixture is then stirred for about 18 hr. with cooling in an ice bath. It is then poured onto a mixture of ice, water and concentrated hydrochloric acid and stirred for 0.5 hr., and the nitrobenzene layer is separated. The nitrobenzene is removed by steam distillation and the residue is crystallised from a small volume of ethanol to constant melting point.

후처리

  1. addition36211/75), is added in drops
  2. temperaturewith cooling in an ice bath
  3. stirringstirred for 0.5 hr
  4. custom, and the nitrobenzene layer is separated
  5. customThe nitrobenzene is removed by steam distillation
  6. customthe residue is crystallised from a small volume of ethanol to constant melting point

출처 및 근거

ORD 기록
ord-d8bd9553888746338d44dceea6760389
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04149413

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