HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 66616333, compound → HCID 16062389, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 66616333 | HCID 66616333 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Product | HCID 16062389 | HCID 16062389 | — |
Reaction Steps
A mixture of crude 1-[4-(4-fluoro-phenyl)-2-isopropyl-7,8-dihydro-5H-pyrido[4,3-d]pyrimidin-6-yl]-ethanone in 10% aq. HCl (800 mL) was heated at reflux for 2 h and then cooled to rt. The aqueous solution was washed with EtOAc (400 mL) and then was basified with NaOH pellets (˜120 g) to pH>12. The basic solution was extracted with CH2Cl2 (2×500 mL). The combined organic layers were washed with 1 N NaOH (400 mL), dried (MgSO4), and concentrated to give the crude product (100 g), which was used in the next reaction without further purification. HPLC: RT=6.89 min. MS (ESI): exact mass calcd. for C16H18FN3, 271.15; m/z found, 271.9 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08618288B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-4ac668b6872647628bdd567c9dca40ec |
| Source note | uspto-grants-2013_12 |