Hydrochloric Acid → Ethyl (4-{[5-bromo-4-(methylthio)pyrimidin-2-yl]amino}phenyl)(methyl)oxido-lambda-sulfanylidenecarbamate

(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%).

1. customconsumption of starting sulfoximine
2. additionThe reaction mixture is poured into 800 mL of aq. NaHCO3
3. filtrationthe pasty precipitate filtered
4. washwashed with 70 mL of EtOAc
5. customcrude material (7.5 g) is recrystallized
6. customto yield 6 g (35%)

ORDレコード

ord-609eeef5aea540ccb335561e18c97e31

出典データセット

uspto-grants-2014_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08642611B2