HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → N-(2-(tert-butyldimethylsilyloxy)ethyl)-1,1,1-trifluoropropan-2-amine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | tert-Butyldimethylsilyl chloride | HCID 28928 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | Ethanol, 2-[(2,2,2-trifluoro-1-methylethyl)amino]- | HCID 86725833 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | N-(2-(tert-butyldimethylsilyloxy)ethyl)-1,1,1-trifluoropropan-2-amine | HCID 86725834 | 37,1% |
Reaktionsschritte
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).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09045486B2 |
| Quelldatensatz | uspto-grants-2015_06 |
| ORD ID | ord-4befe3b937804849a6ba97f7d1aedff0 |
| Quellennotiz | uspto-grants-2015_06 |