HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,5-dichloro-N-methylpyrimidin-4-amine → Methyl 4-(5-chloro-4-(methylamino)pyrimidin-2-ylamino)-3-(difluoromethoxy)benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,5-dichloro-N-methylpyrimidin-4-amine | HCID 18981247 | — |
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | Methyl 4-amino-3-(difluoromethoxy)benzoate | HCID 43380209 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | Methyl 4-(5-chloro-4-(methylamino)pyrimidin-2-ylamino)-3-(difluoromethoxy)benzoate | HCID 58539120 | — |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
Methyl 4-amino-3-(difluoromethoxy)benzoate (70 mg), 2,5-dichloro-N-methylpyrimidin-4-amine, 0.1 mL of 4N HCl/dioxane and 1 mL of n-butanol were placed in a microwave vial. The reaction was heated for 30 minutes at 150° C. and monitored by LCMS. The mixture was concentrated and purified by silica gel chromatography to give 100 mg of pure methyl 4-(5-chloro-4-(methylamino)pyrimidin-2-ylamino)-3-(difluoromethoxy)benzoate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08354420B2 |
| Source dataset | uspto-grants-2013_01 |
| ORD ID | ord-b6042110bfca4b9c88137e6c7d8340d9 |
| Source note | uspto-grants-2013_01 |