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Sodium Chloride → Di-[1-(1-Methylcyclohexyloxy)-2,2,6,6-tetramethylpiperidin-4-yl] Sebacate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | tert-Butyl hydroperoxide | HCID 6410 | — |
| 反応物 | Tinuvin 770 | HCID 164282 | — |
| 触媒 | Molybdenum trioxide | HCID 14802 | — |
| 溶媒 | Methylcyclohexane | HCID 7962 | — |
| 生成物 | Di-[1-(1-Methylcyclohexyloxy)-2,2,6,6-tetramethylpiperidin-4-yl] Sebacate | HCID 19768333 | 140.7% |
反応手順
t-Butyl hydroperoxide (70%, 133.9 g, 1.04 mol), methylcyclohexane (250 ml), and sodium chloride (20 g) are agitated in a separatory funnel. The organic layer is dried over magnesium sulfate. The t-butyl hydroperoxidemethylcyclohexane solution is mixed with 50.0 g (104 mmol) of di-(2,2,6,6-tetramethylpiperidin-4-yl) sebacate, 3.0 g of molybdenum trioxide, and 100 ml of methylcyclohexane. The reaction mixture is heated at reflux for 4.5 hours and water is collected in a Dean-Stark trap. The reaction is cooled to room temperature and filtered. The filtrate is concentrated at reduced pressure to obtain an oil which is purified by flash chromatography (silica gel; 19:1 heptane:ethyl acetate) to obtain 51.6 g (72% yield) of a colorless oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05204473 |
| 出典データセット | uspto-grants-1993_04 |
| ORD ID | ord-11708737ad92458586bfb04c20f93784 |
| 出典メモ | uspto-grants-1993_04 |