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Bromide ion → (2-Chloro-5-methoxybenzyl)(triphenyl)phosphonium bromide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Bromide ion | HCID 259 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 1-Chloro-4-methoxy-2-methylbenzene | HCID 458156 | — |
| 反応物 | Nbs aibn | HCID 86630000 | — |
| 溶媒 | Methane, dichloro-, compd. with benzene (1:1) | HCID 23443464 | — |
| 生成物 | (2-Chloro-5-methoxybenzyl)(triphenyl)phosphonium bromide | HCID 85758264 | 76% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07094798B1 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-bfdc92081d604501937dbab0c74fb0e9 |
| 出典メモ | uspto-grants-2006_08 |