HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 24822776, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Cesium carbonate | HCID 10796 | — |
| Reactant | 2,4-Dichloropyrimidine | HCID 77531 | — |
| Reactant | 6-Hydroxy-1-naphthoic acid | HCID 5463800 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 24822776 | HCID 24822776 | — |
Reaction Steps
To a solution of 6-hydroxy-1-naphthoic acid (10.0 g, 53.1 mmol) in DMSO (60 mL) was added Cs2CO3 (51.9 g, 159.4 mmol). Bubbling was evident. The mixture was stirred at RT for 5 min, at which time 2,4-dichloropyrimidine (15.8 g, 16.3 mmol) was added. The reaction was stirred at RT and monitored by LCMS for the disappearance of starting material. EtOAc (1.0 L) was added, and the reaction was filtered to remove solid Cs2CO3. The mixture was extracted with 2N aqueous NaOH. The aqueous layer was washed with EtOAc, then acidified with 6N aqueous HCl to provide a white suspension. Filtration yielded a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08178557B2 |
| Source dataset | uspto-grants-2012_05 |
| ORD ID | ord-1cb34c85f20f41668ddffcbb25ee3c91 |
| Source note | uspto-grants-2012_05 |