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2-Tridecanone → 2,3-Dihydroperimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Tridecanone | HCID 11622 | — |
| 反応物 | 1,8-Diaminonaphthalene | HCID 68067 | — |
| 触媒 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2,3-Dihydroperimidine | HCID 12440965 | 174.3% |
反応手順
A stirred mixture of 26.05 g of 1,8-diaminonaphthalene, 32.66 g of 2-tridecanone, 55 mg of p-toluenesulfonic acid monohydrate, and 250 mL of toluene was heated to reflux under a nitrogen atmosphere using a Dean-Stark trap to remove the water evolved from the reaction for 5 hr. The mixture was then washed with saturated sodium bicarbonate solution, dried over anhydrous potassium carbonate, filtered, and the solvent removed under reduced pressure. The product was distilled to yield 48.86 g of dihydroperimidine intermediate, bp 192°-213° C. at 0.3 to 0.4 torr.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05380635 |
| 出典データセット | uspto-grants-1995_01 |
| ORD ID | ord-e3e45563951a4d36ac60f60d1d047019 |
| 出典メモ | uspto-grants-1995_01 |