Ethyl Acetate → 2-(Methylsulfanyl)pyrimidin-5-ol

To a stirring solution of 2-(methylthio)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidine (from step A) (1.167 g, 4.63 mmol) in THF/H2O (20 mL 1:1) at room temperature under argon was added sodium perborate tetrahydrate (2.137 g, 13.9 mmol). The reaction mixture was stirred at room temperature overnight. The reaction was cooled to room temperature. EtOAc (10 mL) was added to the reaction mixture, which was washed with brine (15 mL×3). Organic phase was dried (MgSO4), filtered and concentrated. The crude product was very insoluble, therefore it was used directly to next step. MS (ESI) 143 (M+H).

1. temperatureThe reaction was cooled to room temperature
2. washwas washed with brine (15 mL×3)
3. dry with materialOrganic phase was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated

ORDレコード

ord-85b7039681764b56b930fd22abf2fe66

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08372837B2