Fluretofene → 4'-Ethenyl-2-fluoro-1,1'-biphenyl

HRID 1283634노트

반응식

HRID 1283634 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[F:15])=[CH:5][CH:4]=1)#[CH:2].[H][H]>[Pd].N1C=CC=CC=1>[F:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[C:6]1[CH:5]=[CH:4][C:3]([CH:1]=[CH2:2])=[CH:8][CH:7]=1

참가 물질

5

반응물 2

HCID 42040FluretofeneHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 194261784'-Ethenyl-2-fluoro-1,1'-biphenyl

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 1049Pyridine용매

실험 절차

1-Ethynyl-4-(2-fluorophenyl)benzene, 29.6 g., was reduced in a Parr Instrument Company Series 3910 Low-Pressure Shaker-Type Apparatus, using 450 ml. of pyridine, and 0.3 g. of five percent palladium on barium sulfate; reduction was carried out at room temperature for 30 minutes and at an initial hydrogen pressure of 30 psig. The reaction mixture was filtered and the filtrate was evaporated in vacuo. The residue was vacuum distilled to give 20.5 g. of solid which was recrystallized from methanol to give 4-(2 -fluorophenyl)-1-vinylbenzene, mp 38°. The material contained traces of pyridine and 1-ethyl-4-(2-fluorophenyl)benzene, as shown by nuclear magnetic resonance analysis. The following elemental analysis was obtained:

후처리

  1. filtrationThe reaction mixture was filtered
  2. customthe filtrate was evaporated in vacuo
  3. distillationdistilled
  4. customto give 20.5 g
  5. customof solid which was recrystallized from methanol

출처 및 근거

ORD 기록
ord-90923561189c4f22a426f7f44cfbbb1d
출처 데이터셋
uspto-grants-1976_08
특허 번호
US03975543

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