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Glycine → N-(p-nitrobenzyloxycarbonyl)glycine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Glycine | HCID 750 | — |
| 反応物 | Water ethanol | HCID 19096565 | — |
| 反応物 | Carbonic acid 4-Nitrophenyl (4-Nitrophenyl)methyl Ester | HCID 21829967 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | N-(p-nitrobenzyloxycarbonyl)glycine | HCID 12187147 | 55.7% |
反応手順
One and one half grams of glycine is slurried in 235 ml of a 80/20 minute of ethyl alcohol/water. To this is added 5.6 ml of triethylamine, solution occurs, followed by 6.36 g of product from Example 254. A precipitate forms and the reaction is stirred overnight at room temperature. The reaction mixture is concentrated in vacuo. The resulting oil is dissolved in water and ethyl alcohol, the pH is adjusted to 1.5 with concentrated hydrochloric acid and the volume is reduced. The reaction mixture is extracted with methylene chloride, the organic layer is washed with water and concentrated in vacuo. The residue is purified by chromatography (Silica gel: ethyl acetate) to give 2.83 g of the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05623081 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-3ec5894e745847e89febf951cf65c25f |
| 出典メモ | uspto-grants-1997_04 |