関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Trilauryl phosphite | HCID 76495 | — |
| 反応物 | 6-tert-Butyl-3-(chloromethyl)-2,4-dimethylphenol | HCID 90131 | — |
| 生成物 | Di-n-dodecyl 4-tert.-butyl-2,6-dimethyl-3-hydroxybenzylphosphonate | HCID 21311762 | — |
反応手順
41 Grams of trilauryl phosphite and 16.1 grams of 6-tert.-butyl-3-chloromethyl-2,4-dimethylphenol were stirred together as a melt at 105° to 110° for 1 hour, followed by 110° to 120° for 2 hours, 120° to 125° for 10 hours and finally at 140° to 145° for 4 hours. The crude was topped in the "ASCO 50" Rotafilm Molecular Still at a wall temperature of 80° to 90° at 1 to 5 microns Hg. pressure to remove most of the by-product dodecyl chloride as well as small amounts of other volatiles. This topping procedure was repeated at a wall temperature of 200° to 210° at the same pressure to remove additional volatiles. The desired product distilled at a wall temperature of 250° to 260° at 1 micron Hg. pressure yielding the desired product as a colorless liquid which solidified to a white solid (m.p. 36° to 42°). (compound 3)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04161473 |
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| 出典データセット | uspto-grants-1979_07 |
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| ORD ID | ord-18e42729892143178e2749574963e9f4 |
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| 出典メモ | uspto-grants-1979_07 |
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