化工社化工社 化学情報印刷レポート · 研究参考用
Dimethylformamide → Boc-Gly-Asp(O-cHex) Man(4-MBzl)
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | N-(tert-butoxycarbonyl)glycine | HCID 78288 | — |
| 反応物 | Asp(O-cHex) Man(4-MBzl) | HCID 131720066 | — |
| 生成物 | Boc-Gly-Asp(O-cHex) Man(4-MBzl) | HCID 131720067 | 89.2% |
反応手順
To a cold solution of Asp(O-cHex)-Man(4-MBzl) (46.7 g, 86.4 mmol) in DMF (100 mL) diisopropylethylamine (15 mL, 86.1 mmol) was added. N-Hydroxybezotriazole (14.0 g, 104 mmol) was added followed by Boc-Gly (16.6 g, 94.8 mmol). The reaction mixture was stirred in the cold for a few minutes, and N-ethyl-N'-(dimethylaminopropyl)carbodiimide (18.2 g, 94.9 mmol) was added. The reaction mixture was allowed to warm to room temperature and stirred for 18 h. The reaction mixture was concentrated to a small volume and poured into 1.5 L of aqueous 10% K2CO3. The precipitated product was collected by filtration and was washed with water to a neutral pH to afford the titled compound (50.6 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05643872 |
| 出典データセット | uspto-grants-1997_07 |
| ORD ID | ord-7b1bd11af3fb4384a90bb41cf3b3cf5c |
| 出典メモ | uspto-grants-1997_07 |