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Benzene, 1,3-bis(chloromethyl)- → 3-(Chloromethyl)benzyltri-n-butylphosphonium chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzene, 1,3-bis(chloromethyl)- | HCID 12275 | — |
| 反応物 | Tributylphosphine | HCID 13831 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 3-(Chloromethyl)benzyltri-n-butylphosphonium chloride | HCID 67656536 | — |
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-m-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, after which time the tri-n-butylphosphonium chloride salt had crystallized out of solution and TLC examination showed completion of reaction. The white crystals were filtered and washed several times with toluene and hexanes, and then dried. 1H NMR (CDCl3) δ 0.93 (t, 9H), 1.45 (m, 12H), 2.41 (m, 6H), 4.40 (d, 2H), 4.57 (s, 2H), 7.36 (m, 2H), 7.42 (d, 2H).
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-ededb267cad641e9a7f04d2a0d38f761 |
| 出典メモ | uspto-grants-1995_09 |