Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 11154830 | HCID 11154830 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 15545159 | HCID 15545159 | 62% |
Reaction Steps
2.0 g of methyl 1-[2-chloro-4-fluoro-5-{3-methyl-2,6-dioxo-4-(trifluoromethyl)-1,2,3,6-tetrahydropyrimidin-1-yl}phenoxy]cyclopropanecarboxylate was dissolved in a solution consisting of 10 ml of 1,4-dioxane and 10 ml of conc. hydrochloric acid, and the obtained solution was heated under reflux for 2 hours. The reaction mixture was poured into ice water and extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride solution in turn, and dried over anhydrous magnesium sulfate. The resultant was concentrated under reduced pressure. The produced crystals was washed with a mixted solution of hexane and t-butyl methyl ether to give 1.2 g of 1-[2-chloro-4-fluoro-5-{3-methyl-2,6-dioxo-4-(trifluoro-methyl)-1,2,3,6-tetrahydropyrimidin-1-yl}phenoxy]cyclo-propanecarboxylic acid (Compound 1-1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06403534B1 |
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| Source dataset | uspto-grants-2002_06 |
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| ORD ID | ord-bc2ea7a6055f4d3bb702eac224a4b20d |
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| Source note | uspto-grants-2002_06 |
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