Reaktion #11182

ord-bfdc92081d604501937dbab0c74fb0e9

Reaktionsgleichung

COc1ccc(Cl)c(C)c1
1-chloro-4-methoxy-2-methylbenzene
CC(C)(C#N)N=NC(C)(C)C#N.O=C1CCC(=O)N1Br
NBS AIBN
[Br-]
bromide
c1ccc(P(c2ccccc2)c2ccccc2)cc1
triphenylphosphine
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
phosphonium
Ausbeute 76.0%
COc1ccc(Cl)c(C[P+](c2ccccc2)(c2ccccc2)c2ccccc2)c1.[Br-]
(2-Chloro-5-methoxybenzyl)(triphenyl)phosphonium bromide
Ausbeute 76.0%

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Vorschrift

Bromination of 1-chloro-4-methoxy-2-methylbenzene with NBS/AIBN, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 102, except that the reaction time for the bromination was 4 h, gave the phosphonium salt (578) (76%) as a light brown solid, mp (CH2Cl2/benzene) 189–190.5° C. 1H NMR (CDCl3) δ 7.82–7.61 (m, 15H), 7.21 (t, J=2.8 Hz, 1H), 7.04 (dd, J=8.8, 0.8 Hz, 1H), 6.76 (dt, J=8.9, 2.7 Hz, 1H), 5.59 (d, J=14.4 Hz, 2H), 3.58 (s, 3H). Found: C, 62.75; H, 4.70. C26H23BrClOP requires-C, 62.73; H, 4.66.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07094798B1uspto-grants-2006_08