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Bromide ion → (2-Chloro-4-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 | Hydrogen Bromide | HCID 260 | — |
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | (2-Chloro-4-methoxyphenyl)methanol | HCID 14771756 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methane, dichloro-, compd. with benzene (1:1) | HCID 23443464 | — |
| 生成物 | (2-Chloro-4-methoxybenzyl)(triphenyl)phosphonium bromide | HCID 87899044 | 100% |
反応手順
Bromination of (2-chloro-4-methoxyphenyl)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 reaction time for the bromination was 4 h and the reaction time for the displacement was 28 h, gave the phosphonium salt (574) (100%) as a white solid, mp (CH2Cl2/benzene) 223–226° C. 1H NMR (CDCl3) δ 7.82–7.61 (m, 15H), 7.53 (dd, J=8.4, 2.7 Hz, 1H), 6.72 (d, J=2.8 Hz, 1H), 6.70 (dd, J=8.9, 2.5 Hz, 1H), 5.57 (d, J=13.6 Hz, 2H), 3.74 (s, 3H). Found: C, 63.05; H, 4.74. 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-b0cc435ca11b4dacb9b6522a9e461fa6 |
| 出典メモ | uspto-grants-2006_08 |