HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → Ethyl (4-{[5-bromo-4-(methylthio)pyrimidin-2-yl]amino}phenyl)(methyl)oxido-lambda-sulfanylidenecarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | 5-Bromo-2-chloro-4-(methylthio)pyrimidine | HCID 12264796 | — |
| Reactant | Ethyl [(4-aminophenyl)(methyl)oxido-sulfanylidene]carbamate | HCID 44122615 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Solvent | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Product | Ethyl (4-{[5-bromo-4-(methylthio)pyrimidin-2-yl]amino}phenyl)(methyl)oxido-lambda-sulfanylidenecarbamate | HCID 50742701 | — |
Reaction Steps
(RS)—S-(4-aminophenyl)-N-(ethoxycarbonyl)-S-methylsulfoximide (10 g, 42 mmol), 5-bromo-2-chloro-4-methylsulfanyl-pyrimidine (10 g, 42 mmol) and 5M HCl (8 mL) in dioxane is stirred at 60° C. in 90% acetonitrile-water (250 mL) for 36 h. TLC indicates almost complete consumption of starting sulfoximine. The reaction mixture is poured into 800 mL of aq. NaHCO3, the pasty precipitate filtered, washed with 70 mL of EtOAc, then crude material (7.5 g) is recrystallized from boiling EtOH (200 mL) to yield 6 g (35%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08524724B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-f8aebceef0dc4f538631836f129f5116 |
| Source note | uspto-grants-2013_09 |