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Triethylamine → N,O-dimethyl-N-(1-trityl-piperidine-4-carbonyl)hydroxylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide | HCID 15908 | — |
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 反応物 | 1-Tritylpiperidine-4-carboxylic acid | HCID 20520182 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N,O-dimethyl-N-(1-trityl-piperidine-4-carbonyl)hydroxylamine | HCID 22628088 | — |
反応手順
To a mixture of 1-tritylpiperidine-4-carboxylic acid (7.0 g), O,N-dimethylhydroxylamine hydrochloride (2.0 g) and triethylamine (2.9 ml) in dichloromethane (70 ml) was added WSC (3.97 g), and the mixture was stirred at room temperature for 1 hour and concentrated. To the residue was added ethyl acetate, and the mixture was washed with water, dried (MgSO4) and concentrated. The resulting crystals (6.3 g) were washed with isopropylether.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06359134B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-13e3f414752049a18edaff60a4782d74 |
| 出典メモ | uspto-grants-2002_03 |