반응 #11244

ord-9d994210277644129c424413fa4c52d0

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITfollowed by 1 day at 55° C.

실험 절차

Bromination of (2-methoxy-4-nitrophenyl)methanol with 30% HBr in acetic acid, followed by reaction of the crude bromide with triphenylphosphine, using the procedure described in example 112, except that the conditions for the displacement were 3 days at 20° C. followed by 1 day at 55° C., gave the phosphonium salt (582) (84%) as a yellow solid, mp (CH2Cl2/benzene) 194–196° C. 1H NMR (CDCl3) δ 7.83–7.63 (m, 17H), 7.45 (br s, 1H), 5.52 (d, J=15.0 Hz, 2H). Found: C, 61.10; H, 4.73; N, 3.05. C26H23BrNO3P requires C, 61.43; H, 4.56; N, 2.76.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07094798B1uspto-grants-2006_08