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N,N-Dimethylcyclohexylamine → 3-Hydroxy-2-cyclobuten-1-one-cyclohexyldimethylammonium salt
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N,N-Dimethylcyclohexylamine | HCID 7415 | — |
| 反応物 | Cyclobutane-1,3-dione | HCID 27357 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 3-Hydroxy-2-cyclobuten-1-one-cyclohexyldimethylammonium salt | HCID 19896032 | 87.4% |
反応手順
A solution of 3.21 g of N,N-dimethylcyclohexylamine (99 percent; 25.0 mmol) in 10 g of ethyl acetate was instilled in a suspension of 2.1 g of 1,3-cyclobutanedione (91.9 percent; 23.0 mmol) in 40 g of ethyl acetate at 20° C. in 15 minutes. After 1 hour of stirring at room temperature, the suspension was filtered and dried under vacuum. 4.27 g of the title product with a purity of 94.8 percent (according to HPLC), corresponding to a yield of 83.3 percent, relative to the cyclobutanedione, was obtained. Data for the title compound was:
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05118847 |
| 出典データセット | uspto-grants-1992_06 |
| ORD ID | ord-301a84d73f9d4c21be048768e7f4a8d3 |
| 出典メモ | uspto-grants-1992_06 |