HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 23284511, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chlorosulfonyl isocyanate | HCID 70918 | — |
| Reactant | HCID 23284475 | HCID 23284475 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 23284511 | HCID 23284511 | 55% |
Reaction Steps
Chlorosulfonyl isocyanate (0.5 ml, 5.6 mmol) was added to a solution of 2-ethylamino-3-(2-thiophenecarbonyl)pyridine (1.01 g, 4.35 mmol) in tetrahydrofuran (50 ml) under ice-cooling, followed by stirring for 30 minutes. The reaction solution was mixed with water and extracted with chloroform. The organic layer was washed with brine and dried over anhydrous sodium sulfate. After removing sodium sulfate by filtration, the resulting filtrate was concentrated under a reduced pressure and the resulting residue was purified by silica gel column chromatography (chloroform-ethyl acetate) and recrystallized from ethyl acetate to give 1-ethyl-4-(2-thienyl)pyrido[2,3-d]pyrimidin-2(1H)-one (613 mg, 2.38 mmol, 55%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06136810 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-99c3efc80eee4bdb8f860f54dae3a034 |
| Source note | uspto-grants-2000_10 |