1,2-Bis(chloromethyl)benzene → HCID 67656234, Verbindung

HRID 265999

Reaktionsgleichung

Reaktionsgleichung von HRID 265999
[CH2:1]([P:5]([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:6][CH2:7][CH2:8][CH3:9])[CH2:2][CH2:3][CH3:4].[Cl:14][CH2:15][C:16]1[C:17]([CH2:22][Cl:23])=[CH:18][CH:19]=[CH:20][CH:21]=1>C1(C)C=CC=CC=1>[Cl-:14].[Cl:23][CH2:22][C:17]1[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=1[CH2:15][P+:5]([CH2:6][CH2:7][CH2:8][CH3:9])([CH2:10][CH2:11][CH2:12][CH3:13])[CH2:1][CH2:2][CH2:3][CH3:4]

Komponenten

4

Edukt 2

HCID 119191,2-Bis(chloromethyl)benzeneHCID 13831Tributylphosphine

Produkt 1

HCID 67656234HCID 67656234, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel2×

Versuchsvorschrift

A mixture of tri-n-butylphosphine (18.9 g, 103.8 mmol) in toluene (50 mL) was added dropwise to a mixture of α,α'-dichloro-o-xylene (7.0 g, 34.6 mmol) in toluene (200 mL) under argon gas. The reaction mixture was allowed to stir for several days at room temperature under argon, at which time TLC examination showed completion of reaction. Toluene was removed under reduced pressure to give an oily residue. The above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL), and then dried to give a colorless oil. 1H NMR (CDCl3) δ 0.89 (t, 9H), 1.43 (m, 12H), 2.52 (m, 6H), 4.41 (d, 2H), 4.88 (s, 2H), 7.33 (m, 2H), 7.45 (m, 1H), 7.52 (m, 1H).

Aufarbeitung

  1. customcompletion of reaction
  2. customToluene was removed under reduced pressure
  3. customto give an oily residue
  4. washThe above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL)
  5. customdried
  6. customto give a colorless oil

Quellen und Nachweise

ORD-Eintrag
ord-cdcffba7dce24911a2e8597c5c20513c
Quelldatensatz
uspto-grants-1997_07
Patentnummer
US05650099

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