Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | HCID 59506448 | HCID 59506448 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59506412 | HCID 59506412 | — |
Reaction Steps
Ethyl 8-benzyl-4-chloro-2-(methylthio)-5-oxo-5,6,7,8-tetrahydropyrido[2,3-d]pyrimidine-6-carboxylate from step-1 (48 g, 0.122 mol) in 1,4-dioxane (300 mL), and triethylamine (20.5 mL, 0.147 mol) was added hydrazine hydrate (6.73 g, 0.134.6 mol). The reaction mixture was stirred at room temperature for 5-6 h. After completion of the reaction, dioxane was evaporated under vacuo, and water (250 mL) was added to the reaction mixture and was extracted with dichloromethane (200 mL×3). The combined dichloromethane layer was washed with water (500 mL) followed by brine (500 mL). The dichloromethane layer was dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to give crude ethyl 8-benzyl-4-hydrazinyl-2-(methylthio)-5-oxo-5,6,7,8-tetrahydropyrido[2,3-d]pyrimidine-6-carboxylate as an oil that was used for next step without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08343983B2 |
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| Source dataset | uspto-grants-2013_01 |
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| ORD ID | ord-4a48caf61ef8438bb256f57dea4498c1 |
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| Source note | uspto-grants-2013_01 |
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