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1,2-Bis(chloromethyl)benzene → 2-(Chloromethyl)benzyltriethylphosphonium 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 | Triethylphosphine | HCID 27365 | — |
| 反応物 | Triethylphosphonium chloride salt | HCID 19032181 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(Chloromethyl)benzyltriethylphosphonium chloride | HCID 19032170 | — |
反応手順
To a mixture of α,α'-dichloro-o-xylene (15.0 g, 86.0 mmol) in toluene (200 ml) was added triethylphosphine (6.3 ml, 43.0 mmol) under argon gas. The reaction mixture was stirred for several days at room temperature under argon after which time the triethylphosphonium chloride salt had crystallized out of solution. The crystals were filtered and washed with toluene (3×50 mL) and pentane (3×50 mL) and dried: 1H NMR (CDCl3) δ1.15-1.26 (dt, 9), 2.58-2.69 (m, 6H), 4.39-4.44 (d, 2H), 4.87 (s, 2H) , 7.31-7.34 (dd, 2H) , 7.43-7.46 (dd, 1H), 7.50-7.54 (m, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05484556 |
| 出典データセット | uspto-grants-1996_01 |
| ORD ID | ord-10ae76f6ec0f4443944228377f5b406d |
| 出典メモ | uspto-grants-1996_01 |