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Phosphorus sulfide (P2S5) → 2,6-Diphenylthiopyrylium perchlorate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| 反応物 | 1,3-Dibenzoylpropane | HCID 80432 | — |
| 反応物 | Lithium perchlorate | HCID 23665649 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2,6-Diphenylthiopyrylium perchlorate | HCID 85615143 | 24% |
反応手順
The 1,5-diphenyl-1,5-pentanedione prepared in step 1 (10 mmol, 2.52 g) is mixed with phosphorus pentasulfide (15 mmol, 3.34 g), acetic acid (60 mL) and lithium perchlorate (60 mmol, 6.40 g) in a 100 mL two-necked round-bottomed flask, and then refluxed for 3 hours. The solution then becomes orange and a white precipitate forms. The precipitate is removed by filtration on a sinter funnel and then washed with hot acetic acid. The solution is concentrated on a rotary evaporator and recrystallized by addition of ether (500 mL). The precipitate obtained is filtered off on a sinter funnel and then dried on a rotary evaporator. The product obtained is a yellow solid in a mass of 850 mg. The reaction yield is 24%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08383931B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-acea0814511143e5916fdb418c642130 |
| 出典メモ | uspto-grants-2013_02 |