HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Morpholine → HCID 178493888, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Morpholine | HCID 8083 | — |
| Edukt | 2-Methylnicotinic acid | HCID 643373 | — |
| Edukt | (S)-glycidyl methanesulfonate | HCID 12461090 | — |
| Edukt | HCID 178493879 | HCID 178493879 | — |
| Lösungsmittel | Methanol | HCID 887 | — |
| Lösungsmittel | Dichloromethane methanol | HCID 21226129 | — |
| Produkt | HCID 178493888 | HCID 178493888 | — |
Reaktionsschritte
Prepared using (S)-glycidyl methanesulfonate (Intermediate H, Step 1) in place of (R)-glycidyl methanesulfonate (Intermediate F, Step 1), and morpholine in place of piperidine in Step 1, and 2-methyl-3-pyridinecarboxylic acid in place of nicotinic acid in Step 2 (0.059 g, 56%): TLC (9:1 CH2Cl2/MeOH+1% NH4OH in MeOH)Rf 0.44; HPLC ret. time 0.81 min.; 1H NMR (DMSO-d6+1 drop TFA-d) δ 2.99 (s, 3H), 3.09-3.40 (m, 4H), 3.48 (br d, J=12.1 Hz, 2H), 3.63-3.83 (m, 2H), 3.89-4.01 (m, 2H), 4.02 (s, 3H), 4.18-4.29 (m, 4H), 4.38-4.46 (m, 1H), 4.46-4.55 (m, 2H), 7.50 (d, J=9.0 Hz, 1H), 7.96 (dd, J=6.2, 7.5 Hz, 1H), 8.05 (d, J=9.0 Hz, 1H), 8.91 (d, J=5.5 Hz, 1H), 9.06 (br d, J=8.3 Hz, 1H); mass spectrum m/z 495 ((M+1)+, 2.3%).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08895549B2 |
| Quelldatensatz | uspto-grants-2014_11 |
| ORD ID | ord-68442aeb13d748458fb44612f4570eb0 |
| Quellennotiz | uspto-grants-2014_11 |