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

HRID 26336

反応式

HRID 26336 の反応式
[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]

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7416Nitrobenzene溶媒

反応条件

温度
-7 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d8bd9553888746338d44dceea6760389
出典データセット
uspto-grants-1979_04
特許番号
US04149413

関連ノート

読み込み中…