HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
4-Methylmorpholine → Pyridine-2-sulfonic acid allyl-(2-methyl-pent-4enyl)-amide
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 4-Methylmorpholine | HCID 7972 | — |
| Edukt | Pyridine-2-sulfonyl Chloride | HCID 3787675 | — |
| Edukt | Allyl-(2-methyl-pent-4-enyl)-amine | HCID 11378535 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | Pyridine-2-sulfonic acid allyl-(2-methyl-pent-4enyl)-amide | HCID 11565389 | 60% |
Reaktionsschritte
Allyl-(2-methyl-pent-4-enyl)-amine (1.0 g, 7.2 mmol) and NMM (1.7 g, 17.2 mmol) were mixed in 30 ml CH2Cl2. 2-pyridinesulphonyl chloride (1.53 g, 8.6 mmol) was added slowly to the solution while it was cooled in an ice-water bath. After addition, the reaction mixture was stirred at RT overnight. The reaction mixture was washed with 10% NaHCO3 and the brine, then was purified by column chromatography to give the title compound as a colorless oil (1.2 g ,60% yield): MS (M+H+) 281.2; 1H-NMR (400 Hz, CDCl3): d=8.70(d, 1H), 8.0–7.75(m, 2H), 7.5 (m, 1H) 5.80–5.60(m, 2H), 5.15–4.92(m, 4H), 4.00–3.90(m, 2H), 3.20–3.06(m, 2H), 2.15(m, 1H), 1.85(m, 2H), 0.89(d, 3H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07071184B2 |
| Quelldatensatz | uspto-grants-2006_07 |
| ORD ID | ord-641d6ec4383d4f94a02c686482e313a0 |
| Quellennotiz | uspto-grants-2006_07 |