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Bromide ion → (2,6-Dibromobenzyl)(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 | 2,6-Dibromotoluene | HCID 34681 | — |
| 反応物 | Nbs aibn | HCID 86630000 | — |
| 溶媒 | Methane, dichloro-, compd. with benzene (1:1) | HCID 23443464 | — |
| 生成物 | (2,6-Dibromobenzyl)(triphenyl)phosphonium bromide | HCID 87899089 | 95% |
反応手順
Bromination of 2,6-dibromotoluene 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 3 h, gave the phosphonium salt (516) (95%) as a cream powder, mp (CH2Cl2/benzene) 241–243° C. 1H NMR (CDCl3) δ 7.78 (m, 9H), 7.64 (m, 6H), 7.40 (br d, J=7.9 Hz, 2H), 6.99 (td, J=8.0, 2.5 Hz, 1H), 5.58 (d, J=14.1 Hz, 2H). Found: C, 47.06; H, 3.37. C25H20Br3P.3/4 CH2Cl2 requires C, 47.23; H, 3.31.
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-62d61bd7e7f844569eafefc807ca8df6 |
| 出典メモ | uspto-grants-2006_08 |