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Succinic Acid → N-trityl piperazine, succinate salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Succinic Acid | HCID 1110 | — |
| 反応物 | Piperazine | HCID 4837 | — |
| 反応物 | Trityl chloride | HCID 6456 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 溶媒 | Toluene methanol | HCID 21867641 | — |
| 生成物 | N-trityl piperazine, succinate salt | HCID 67005131 | 70% |
反応手順
To a cooled solution of piperazine (10 eq) in toluene/methanol (5:1 toluene/methanol (v:v); 5 mL/g piperazine) was added slowly a solution of trityl chloride 10 (1.0 eq) in toluene (5 mL/g trityl chloride). Upon reaction completion (1-2 hr), this solution was washed four times with water. To the resulting organic solution was added an aqueous solution of succinic acid (1.1 eq; 13 mL water/g succinic acid). This mixture was stirred for 90 min, and the solid product was collected by filtration. The crude solid was purified by two reslurries in acetone. Yield=70%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536147B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-88f9cb7427b947d982fa3667e71af104 |
| 出典メモ | uspto-grants-2013_09 |