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1,2-Bis(chloromethyl)benzene → 2-(Chloromethyl)benzyltri-n-butylphosphonium chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Bis(chloromethyl)benzene | HCID 11919 | — |
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(Chloromethyl)benzyltri-n-butylphosphonium chloride | HCID 67656234 | — |
反応手順
A mixture of tri-n-butylphosphine (18.9 g, 103.8 mmol) in toluene (50 mL) was added dropwise to a mixture of α,α'-dichloro-o-xylene (7.0 g, 34.6 mmol) in toluene (200 mL) under argon gas. The reaction mixture was allowed to stir for several days at room temperature under argon, at which time TLC examination showed completion of reaction. Toluene was removed under reduced pressure to give an oily residue. The above oily residue was washed with toluene/hexane (50/50 (v/v), 4×100 mL), and then dried to give a colorless oil. 1H NMR (CDCl3) δ 0.89 (t, 9H), 1.43 (m, 12H), 2.52 (m, 6H), 4.41 (d, 2H), 4.88 (s, 2H), 7.33 (m, 2H), 7.45 (m, 1H), 7.52 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05451347 |
| 出典データセット | uspto-grants-1995_09 |
| ORD ID | ord-f2a7d95f680842c6892208dfba32a576 |
| 出典メモ | uspto-grants-1995_09 |