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Bromide ion → (2,6-Dichloro-3-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 | (2,6-Dichloro-3-methoxyphenyl)methanol | HCID 21980844 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methane, dichloro-, compd. with benzene (1:1) | HCID 23443464 | — |
| 生成物 | (2,6-Dichloro-3-methoxybenzyl)(triphenyl)phosphonium bromide | HCID 87899066 | 97% |
反応手順
Bromination of (2,6-dichloro-3-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 displacement was 36 h, gave the phosphonium salt (526) (97%) as a white solid, mp (CH2Cl2/benzene) 242–244° C. 1H NMR (CDCl3) δ 7.83–7.60 (m, 15H), 7.15 (dd, J=9.1, 0.8 Hz, 1H), 6.88 (dd, J=9.0, 2.4 Hz, 1H), 5.41 (d, J=14.3 Hz, 2H), 3.84 (s, 3H). Found: C, 58.68; H, 4.16. C26H22BrCl2OP requires C, 58.67; H, 4.17.
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-45cd2ce8b12c4a538ef3a33a64d2aec4 |
| 出典メモ | uspto-grants-2006_08 |