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2-(3'-tert-Butyl-2'-hydroxy-5'-(2-methoxycarbonylethyl)phenyl)benzotriazole → N-(1-Octyloxy-2,2,6,6-tetramethylpiperidin-4-yl)-3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(3'-tert-Butyl-2'-hydroxy-5'-(2-methoxycarbonylethyl)phenyl)benzotriazole | HCID 93481 | — |
| 反応物 | 4-Amino-N-octyloxy-2,2,6,6-tetramethylpiperidine | HCID 23372093 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(1-Octyloxy-2,2,6,6-tetramethylpiperidin-4-yl)-3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamamide | HCID 21645439 | 15% |
反応手順
A mixture of 4.0 g (11.3 mmol) of methyl 3-(2H-benzotriazol-2-yl)-5-tert-butyl-4-hydroxyhydrocinnamate and 8.0 g (28.1 mmol) of 4-amino-1-octyloxy-2,2,6,6-tetramethylpiperidine is heated at 190°-200° C. for 2 hours. The reaction mixture is dissolved in ethyl acetate (300 ml). The organic solution is washed with 1N hydrochloric acid (2 ×100 ml) and saturated sodium bicarbonate solution (200 ml), then dried over magnesium sulfate and evaporated to obtain a solid. Purification by flash chromatography on silica gel (3:1 heptane: ethyl acetate) following by recrystallization from methanol affords 1.0 g (15% yield) of the title compound, a white solid, mp 153°-9° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05021478 |
| 出典データセット | uspto-grants-1991_06 |
| ORD ID | ord-62193cd13d364ebcb097d26237458510 |
| 出典メモ | uspto-grants-1991_06 |