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Tetrahydrofuran → N-(cholest-5-ene-3beta-oxycarbonyl)glycylglycine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Glycylglycine | HCID 11163 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | C28H45ClO2 | HCID 54236888 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(cholest-5-ene-3beta-oxycarbonyl)glycylglycine | HCID 131717552 | 80.8% |
反応手順
Sodium hydrogencarbonate (0.168 g) and tetrahydrofuran (20 ml) were added to a suspension of glycylglycine (0.15 g) in water (20 ml). After tetrahydrofuran (20 ml) and cholesteryl chloroformate (0.898 g) were added to the resulting transparent solution at 0° C., the mixture was stirred for an hour. The reaction mixture was concentrated under reduced pressure and, methanl (10 ml) and chloroform (10 ml) were added to the residue. By filtration, the transparent solution was obtained. The solvent was distilled off to give crude crystals (0.98 g). The crude crystals were then purified by silica gel chromatography to give N-(cholest-5-ene-3β-oxycarbonyl)glycylglycine (0.5 g) as white powders.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05152999 |
| 出典データセット | uspto-grants-1992_10 |
| ORD ID | ord-c01942f2ad344ee7b3deac1007c75775 |
| 出典メモ | uspto-grants-1992_10 |