関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Methyl Methacrylate | HCID 6658 | — |
| 反応物 | Phenothiazine | HCID 7108 | — |
| 反応物 | 2-(2-(Dimethylamino)ethoxy)ethanol | HCID 74348 | — |
| 反応物 | Magnesium | HCID 5462224 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-(2-Dimethylaminoethoxy)ethyl Methacrylate | HCID 15870290 | — |
反応手順
A magnesium methoxide solution was prepared by dissolving magnesium metal (4 g) in anhydrous methanol (100 ml) in the presence of a small amount of iodine (approximately 0.1 g). A portion of the resulting solution (18 ml) was placed in a 250 ml reaction vessel and then 2-(2-dimethylaminoethoxy)ethanol (23.6 g) was added, followed by the addition of phenothiazine (0.1 g) and methyl methacrylate (117 g). The mixture was stirred and heated until the methanol started to distill. When all of the methanol was collected, the mixture was cooled to room temperature and the solids were filtered off. The filtrate was subjected to fractionation under reduced pressure. The excess of methyl methacrylate was separated and then pure 2-(2-dimethylaminoethoxy)ethyl methacrylate was collected at 97-102° C./4 mmHg. Yield 22.1 g.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05925253 |
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| 出典データセット | uspto-grants-1999_07 |
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| ORD ID | ord-d1ed5f33d9364e8cb4ab1b7b339ae5e7 |
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| 出典メモ | uspto-grants-1999_07 |
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