関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Methacryloyl chloride | HCID 13528 | — |
| 反応物 | L-Lysine monohydrochloride | HCID 69568 | — |
| 反応物 | Potassium Bicarbonate | HCID 516893 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Lysine-methacrylamide | HCID 88031551 | — |
反応手順
Potassium hydrogencarbonate(5.51 g) was dissolved in 100 ml of distilled water, 9.13 g of lysine hydrochloride was dissolved in the solution, and 80 ml of acetone was further added to the solution. The reaction mixture was added dropwise with 5.23 g of methacryloyl chloride over about 10 minutes with vigorous stirring under ice cooling, and further vigorously stirred for about 2 hours. The reaction mixture was adjusted to pH 1-2 with concentrated hydrochloric acid, and saturated with sodium chloride. The aqueous layer was washed twice with 100 ml of ethyl acetate, and extracted 3 times with 100 ml of ethyl acetate/isopropanol=1/2. The ethyl acetate/isopropanol layers were combined, concentrated to about 50 ml under reduced pressure, added with 500 ml of isopropanol, and again concentrated to about 200 ml. The deposited sodium chloride was removed by filtration, and the filtrate was concentrated (colorless syrup, 5.53 g)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06703468B1 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-744101f63a93452bb2a11a400eabb871 |
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| 出典メモ | uspto-grants-2004_03 |
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