HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Imidazole → HCID 59193319, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Imidazole | HCID 795 | — |
| Edukt | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Edukt | Salicyloyl chloride | HCID 74041 | — |
| Edukt | N-(tert-Butoxycarbonyl)-N'-methylethylenediamine | HCID 3435744 | — |
| Lösungsmittel | Ethyl Acetate | HCID 8857 | — |
| Produkt | HCID 59193319 | HCID 59193319 | 34% |
Reaktionsschritte
To a mixture of tert-butyl 2-(methylamino)ethylcarbamate (0.348 g, 2 mmol), 2-hydroxybenzoyl chloride (0.276 g, 2 mmol) and imidazole (0.136 g, 2 mmol) in ethyl acetate (8 mL) at 0° C. was slowly added a solution of DCC (0.412 g, 2 mmol) in ethyl acetate (2 mL). The mixture was stirred (RT, 16 h), filtered and concentrated under reduced pressure. The crude material was purified by chromatography on silica gel, eluting with EtOAc/PE (20-50%) to afford tert-butyl 2-(2-hydroxy-N-methylbenzamido)ethylcarbamate (0.2 g, 34%) as a colorless oil. 1HNMR (CDCl3): δ 7.5 (m, 2H, CH), 7.0 (d, 1H, CH), 6.8 (d, 1H, CH), 3.7 (m, 2H, CH2), 3.48 (m, 2H, CH2), 3.2 (m, 3H, CH3), 1.5 (s, 9H, CH3).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08846972B2 |
| Quelldatensatz | uspto-grants-2014_09 |
| ORD ID | ord-d8c38b67fdc74d2c9c3c823cfb59ea53 |
| Quellennotiz | uspto-grants-2014_09 |