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N,N-二甲基甲酰胺 → Boc-Gly-Asp(O-cHex) Man(4-MBzl)
参与物
| 角色 | 名称 | HCID | 投料 |
|---|---|---|---|
| 反应物 | N,N-二甲基甲酰胺 | HCID 6228 | — |
| 反应物 | 1-(3-二甲基氨基丙基)-3-乙基碳二亚胺 | HCID 15908 | — |
| 反应物 | 1-羟基苯并三唑(HOBT) | HCID 75771 | — |
| 反应物 | BOC-甘氨酸 | HCID 78288 | — |
| 反应物 | Asp(O-cHex) Man(4-MBzl) | HCID 131720066 | — |
| 产物 | Boc-Gly-Asp(O-cHex) Man(4-MBzl) | HCID 131720067 | 89.2% |
反应步骤
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).
来源与证据
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 专利号 | US05726192 |
| 来源数据集 | uspto-grants-1998_03 |
| ORD ID | ord-bcef87ed7a7043ef86ee001ff10769ae |
| 来源说明 | uspto-grants-1998_03 |