Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Ethylparaben | HCID 8434 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2,4-Dichloro-5-nitropyrimidine | HCID 521266 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 58247411 | HCID 58247411 | — |
Reaction Steps
To a suspension of Compound 1a (2.0 g; 10.31 mmol) and 0.5N NaHCO3 (20 mL; 10 mmol) in acetone (60 mL) was added a solution of 4-hydroxy-benzoic acid ethyl ester (1.71 g; 10.29 mmol) in acetone (20 mL) dropwise at 0° C. The mixture was stirred at 0° C. for 1 h. The reaction mixture was concentrated under reduced pressure. The resultant residue was extracted with EtOAc (2×20 mL). The organic layer was washed with brine and dried over MgSO4 and concentrated. The crude product was purified by normal phase chromatography (SiO2) to give Compound 16a. 1H NMR (300 MHz, CDCl3): δ 9.20 (s, 1H), 8.20 (d, 2H), 7.25 (d, 2H), 4.45 (q, 2H), 1.4 (t, 3H); MS: m/z 324.1 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08685990B2 |
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| Source dataset | uspto-grants-2014_04 |
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| ORD ID | ord-bb82d8825d794362808ff161c8e988e0 |
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| Source note | uspto-grants-2014_04 |
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