Ethyl diphenylphosphinite → 2-(Diphenylphosphinylmethyl)-4'-fluoro-3,5,3'-trimethylbiphenyl

HRID 323570

Reaktionsgleichung

Reaktionsgleichung von HRID 323570
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH3:17])[C:9]=2[CH2:10]Cl)=[CH:4][C:3]=1[CH3:18].C([O:21][P:22]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)C>>[C:23]1([P:22]([CH2:10][C:9]2[C:12]([CH3:17])=[CH:13][C:14]([CH3:16])=[CH:15][C:8]=2[C:5]2[CH:6]=[CH:7][C:2]([F:1])=[C:3]([CH3:18])[CH:4]=2)([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[O:21])[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

Komponenten

3

Edukt 2

HCID 69754Ethyl diphenylphosphiniteHCID 133169812-(4-Fluoro-3-methyl-phenyl)-4,6-dimethylbenzyl chloride

Produkt 1

HCID 154316922-(Diphenylphosphinylmethyl)-4'-fluoro-3,5,3'-trimethylbiphenyl

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

2.06 grams (7.84 mmol) of 2-(4-fluoro-3-methyl-phenyl)-4,6-dimethylbenzyl chloride was treated with ethyldiphenylphosphinite (2.08 grams, 9.01 mmol) and heated to 150° C. for 3 hrs. After cooling to room temperature, the crude mixture was purified by silicagel chromatography ((10% acetone/90% methylene chloride) and the appropriate fractions concentrated and recrystallized from ether/hexane to provide the title compound (MP 109-111° C.).

Aufarbeitung

  1. temperatureAfter cooling to room temperature
  2. customthe crude mixture was purified by silicagel chromatography ((10% acetone/90% methylene chloride)
  3. concentrationthe appropriate fractions concentrated
  4. customrecrystallized from ether/hexane

Quellen und Nachweise

ORD-Eintrag
ord-7379133e361a446da1d4cc45eb76898d
Quelldatensatz
uspto-grants-2001_04
Patentnummer
US06214810B1

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