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Bromide ion → (2-Methoxy-4-nitrobenzyl)(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-Methoxy-4-nitrobenzyl alcohol | HCID 10487701 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Methane, dichloro-, compd. with benzene (1:1) | HCID 23443464 | — |
| 生成物 | (2-Methoxy-4-nitrobenzyl)(triphenyl)phosphonium bromide | HCID 87898968 | 84% |
反応手順
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.
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-9d994210277644129c424413fa4c52d0 |
| 出典メモ | uspto-grants-2006_08 |