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Imidazole → 2-(tert-butyldiphenylsilyloxy)-N-methylethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Imidazole | HCID 795 | — |
| 反応物 | 2-(Methylamino)ethanol | HCID 8016 | — |
| 反応物 | tert-Butyldiphenylchlorosilane | HCID 94078 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-(tert-butyldiphenylsilyloxy)-N-methylethanamine | HCID 11823158 | 31.1% |
反応手順
To a solution of N-methylethanolamine (600 mg), in N,N-dimethylformamide were added imidazole (1.13 g) and tert-butyldiphenylsilyl chloride (2.20 g) at ambient temperature with stirring. After 8 hours, the mixture was diluted with water (60 ml) and was extracted with ethyl acetate (20 ml) twice. The organic layer was washed with water three times and brine, dried over magnesium sulfate. The solvent was removed in vacuo. The residue was purified by column chromatography eluting with dichloromethane-methanol to give N-(2-tert-butyldiphenylsilyloxyethyl)-N-methylamine (780 mg) as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06169095A |
| 出典データセット | uspto-grants-2001_01 |
| ORD ID | ord-12efae263eca4be991f2e94a41bf1af9 |
| 出典メモ | uspto-grants-2001_01 |