関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | [(2R,3R,4R,5R)-3,4-diacetoxy-5-(2-bromo-5,6-dichloro-benzimidazol-1-yl)tetrahydrofuran-2-yl]methyl acetate | HCID 466020 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 溶媒 | Methanol--water (1/1) | HCID 22242641 | — |
| 生成物 | Maribavir Impurity 57 | HCID 22876558 | — |
反応手順
A mixture of 52a (1.048 g, 2.0 mmol) and KOAc (0.98 g, 10.0 mmol) in MeOH/H2O (40 mL/4 mL) was stirred at room temperature for 24 hr. AcOH (0.572 mL, 10.0 mmol) was added and stirring was continued at room temperature for 15 min. The reaction mixture was evaporated and the residue was partitioned between EtOAc/H2O (75 mL/75 mL). The EtOAc layer was washed with sat. NaCl solution (75 mL), dried (Na2SO4), and evaporated. The residue was chromatographed on a silica column (1.9×24 cm, eluted with CHCl3, 2%, 3%, 4% MeOH/CHCl3). Evaporation of fractions 15-27 (15 mL per fraction) and recrystallization from MeOH gave 0.50 g (2 crops, 57%) of 52b as white crystals. MP: 85°-95° C. (melted slowly over a large range) MS: (EI) m/e 437.9398 (15%, M+ =437.9385).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05646125 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-927e1d509b6c4ec89c5fc91f5211e5f0 |
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| 出典メモ | uspto-grants-1997_07 |
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