関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methyl L-phenylalaninate hydrochloride | HCID 75736 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | (S)-Benzyl (tetrahydro-2,5-dioxo-3-furyl)carbamate | HCID 11128682 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | N-(Benzyloxycarbonyl)-L-aspartyl-L-phenylalanine methyl ester | HCID 10159630 | 72.9% |
反応手順
In 100.4 g of acetic acid, 25.1 g (0.1 mole) of N-benzyloxycarbonyl-L-aspartic anhydride was suspended and 21.6 g (0.1 mole) of L-phenylalanine methyl ester hydrochloride was added with stirring at 5°-10° C. Successively 9.2 g (0.1 mole) of sodium acetate was added at the same temperature. The reaction was carried out for 4 hours with stirring at the same temperature. Thereafter 87.1 g of water was added to the reaction mixture to adjust the concentration of organic carboxylic acid to 53.5% by weight. After cooling to 0°-5° C., precipitated crystals were filtered, washed and dried. Crystals of N-benzyloxycarbonyl-α-L-aspartyl-L-phenylalanine methyl ester were obtained The yield was 31.2 g (72.9% yield on L-phenylalanine methyl ester hydrochloride).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05302743 |
|---|
| 出典データセット | uspto-grants-1994_04 |
|---|
| ORD ID | ord-94e87a1b40584184b0aa120578dd7fe6 |
|---|
| 出典メモ | uspto-grants-1994_04 |
|---|