HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67275454, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dichloromethane methanol | HCID 21226129 | — |
| Reactant | HCID 67275522 | HCID 67275522 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 67275454 | HCID 67275454 | — |
Reaction Steps
A solution of EXAMPLE 244B (0.027 g) in trifluoroacetic acid (2 mL) was heated at 75° C. for 18 hours, and concentrated with a toluene azeotrope; and the residue was purified on a reverse phase HPLC on a C8 column with 10-95% acetonitrile in water containing 0.1% trifluoroacetic acid to provide an oily compound. A solution of the oily compound in 1:1 of methanol/dichloromethane was treated with 2N HCl in diethyl ether (0.5 mL), and concentrated. NMR (DMSO-d6) δ ppm 13.34 (m, 1H), 9.72 (bs, 2H), 8.51 (d, 1H), 8.05 (d, 1H), 7.63 (m, 2H), 7.44 (m, 3H), 4.74 (bs, 1H), 4.40-4.00 (m, 5H), 3.70 (m, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08163769B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-38f1a5d98cb04f42b9537084d2282fd1 |
| Source note | uspto-grants-2012_04 |