関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | (+/-)-cis-6-(Cyanomethyl)-1,3-dioxane-4-acetic acid | HCID 15045148 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (+/-)-cis-6-(2-Aminoethyl)-1,3-dioxane-4acetic acid | HCID 15045150 | 60.6% |
反応手順
A solution of 1.04 g (4.88 mmol) of (±)-cis-6-(cyanomethyl)-1,3-dioxane-4-acetic acid in 100 mL of methanol saturated with anhydrous ammonia is added to a Parr shaker bottle containing 0.53 g of water wet Raney nickel #30. The solution is heated at 45° C. and 50 pounds per square inch gage (psig) hydrogen pressure for 17 hours. The suspension is cooled and filtered to remove the Raney nickel through filter aid and the precipitate washed with methanol. The filtrate is concentrated at reduced pressure. The residue is dissolved in methanol saturated with anhydrous ammonia, treated with decolorizing charcoal, filtered through filter aid and evaporated to give 0.56 g of (±)-cis-6-(2-aminoethyl)-1,3-dioxane-4-acetic acid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05216174 |
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| 出典データセット | uspto-grants-1993_06 |
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| ORD ID | ord-4f6fb8f5ab404f4f99d97d07ed54b86d |
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| 出典メモ | uspto-grants-1993_06 |
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