化工社化工社 化学情報印刷レポート · 研究参考用
Water → Methyl alpha,alpha-Dimethyl-9-nitro-9,10-dihydroanthracene-10-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | 9-Nitroanthracene | HCID 11767 | — |
| 反応物 | S-Methyl methanethiosulfonate | HCID 18064 | — |
| 反応物 | Tris(dimethylamino)sulfonium difluorotrimethylsilicate | HCID 9795567 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | Methyl alpha,alpha-Dimethyl-9-nitro-9,10-dihydroanthracene-10-acetate | HCID 13507921 | — |
反応手順
A solution of 1.115 g (5 mmol) of 9-nitroanthracene and 1.01 mL (5 mmol) of MMTS in 20 mL of anhydrous THF was treated with 1.375 g (5 mmol) of TASF dissolved in 3 mL of acetonitrile at -78° C. After addition of TASF had been completed, the reaction mixture was brought to -10° C. and stirred for 1 hr. Ten mL of water was then added, the mixture was warmed to room temperature, and the product was extracted into ether. The organic layer was washed with saturated sodium chloride solution, dried and concentrated. The melting point was 159° to 163° C. (dec). The product material was analyzed by ultraviolet absorption, infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectrometry.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04659862 |
| 出典データセット | uspto-grants-1987_04 |
| ORD ID | ord-f95d76ad56e54d6bb7abcc7ba8eaf04e |
| 出典メモ | uspto-grants-1987_04 |