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1-Hydroxybenzotriazole → HCID 67180248、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 3-(((tert-Butoxycarbonyl)amino)methyl)benzoic acid | HCID 2755929 | — |
| 反応物 | 6-(4-Fluorophenyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine | HCID 69078154 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | HCID 67180248 | HCID 67180248 | 89.8% |
反応手順
To a solution of 6-(4-fluorophenyl)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine (0.20 g) obtained in Reference Example 13C, 1-hydroxy-1H-benzotriazole (0.15 g), triethylamine (0.083 g) and 3-(tert-butoxycarbonylaminomethyl)benzoic acid (0.205 g) in acetonitrile (10 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.314 g), and the mixture was stirred at room temperature for 20 hrs. Ethyl acetate was added to the reaction mixture, and the mixture was washed with water, and dried over anhydrous magnesium sulfate. The solvent was evaporated and the residue was purified by silica gel column chromatography to give the title compound (0.35 g) as a colorless amorphous powder.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07625887B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-43c476ba5ce64a4b9cf6588523737150 |
| 出典メモ | uspto-grants-2009_12 |