HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 69275117, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | Ethanol, mixt. with methanol | HCID 18681192 | — |
| Reactant | HCID 69273627 | HCID 69273627 | — |
| Solvent | Heptane | HCID 8900 | — |
| Product | HCID 69275117 | HCID 69275117 | — |
Reaction Steps
Example 52 (34 mg) was separated from the racemic mixture (80 mg) of Example 51 using a preparative HPLC equipped with a Chiralpak® AD column (5 cm×50 cm, 20μ). The separations were performed using an isocratic method of 95% 1:1 ethanol/methanol, 5% heptane with 0.1% diethylamine for 120 min with a flow rate of 50 mL/min. Retention time for Example 52 was 26 min. Retention time for the other isomer (32 mg) was 90 min. 1H NMR (400 MHz, Methanol-d4) δ ppm 1.33 (m, 9H) 3.01 (m, 3H) 3.98 (m, 2H) 4.59 (m, 3H) 5.61 (d, J=9.54 Hz, 1H) 6.70 (m, 2H) 7.05 (m, 6H) 7.25 (m, 3H) 7.39 (dd, J=12.96, 6.60 Hz, 1H) 7.95 (m, 1H). LC-MS 499 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07456195B2 |
| Source dataset | uspto-grants-2008_11 |
| ORD ID | ord-e82d804de9d54f66bd5bf7f38a9a4aeb |
| Source note | uspto-grants-2008_11 |