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1-Butanol → HCID 178450655、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Urea | HCID 1176 | — |
| 反応物 | Methyl 4-Formylbenzoate | HCID 15294 | — |
| 反応物 | 1,1,4,4-Tetramethyl-6-ethynyl-1,2,3,4-tetrahydronaphthalene | HCID 14726549 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | HCID 178450655 | HCID 178450655 | — |
反応手順
21 g (0.1 mole) of 6-ethynyl-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene, 16 g (0.1 mole) of methyl 4-formylbenzoate, 9 g (0.15 mole) of urea and 15 ml of concentrated sulfuric acid in 50 ml of n-butanol were refluxed for 4 hours. After cooling, the mixture was poured onto 500 ml of water, 100 ml of ether were added and stirring was carried out for 5 minutes. A solid was precipitated between phases. In a shaking funnel, the aqueous phase was separated off and the residue was again washed with water and then shaken thoroughly with 200 ml of petroleum ether. The precipitate was filtered off under suction and washed with petroleum ether. 6.5 g of the title compound of melting point 267°-277° C. were obtained in this manner.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05061705 |
| 出典データセット | uspto-grants-1991_10 |
| ORD ID | ord-5db870c3a531410889b630b942b2bf38 |
| 出典メモ | uspto-grants-1991_10 |