化工社化工社 化学情報印刷レポート · 研究参考用
Water → N-(2-(tert-butyldimethylsilyloxy)ethyl)-1,1,1-trifluoropropan-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Ethanol, 2-[(2,2,2-trifluoro-1-methylethyl)amino]- | HCID 86725833 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-(2-(tert-butyldimethylsilyloxy)ethyl)-1,1,1-trifluoropropan-2-amine | HCID 86725834 | 37.1% |
反応手順
To a stirred solution of 2-(1,1,1-trifluoropropan-2-ylamino)ethanol (40) (5.50 g, 35.0 mmol, Eq: 1.00) in dichloromethane (100 ml) were added diisopropylethylamine (6.33 g, 8.56 ml, 49.0 mmol, Eq: 1.4) followed by tert-butyldimethylsilyl chloride (5.8 g, 38.5 mmol, Eq: 1.1) at room temperature under a nitrogen atmosphere. The resulting solution was stirred for 16 hrs and then it was poured into water (100 ml) and the organic layer was separated, washed with brine, dried (MgSO4), concentrated, and chromatographed (silica gel, gradient 0 to 10% ethyl acetate-hexane) to obtain N-(2-(tert-butyldimethylsilyloxy)ethyl)-1,1,1-trifluoropropan-2-amine (41) (oil, 3.52 g, 13.0 mmol, 37.1% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09045486B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-4befe3b937804849a6ba97f7d1aedff0 |
| 出典メモ | uspto-grants-2015_06 |