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Ethyl Acetate → 2-(Methylsulfanyl)pyrimidin-5-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 2-(Methylthio)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyrimidine | HCID 16414219 | — |
| 反応物 | Sodium;3-oxidodioxaborirane;tetrahydrate | HCID 23693097 | — |
| 溶媒 | Oxolane--water (1/1) | HCID 21881883 | — |
| 生成物 | 2-(Methylsulfanyl)pyrimidin-5-ol | HCID 588357 | — |
反応手順
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).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08372837B2 |
| 出典データセット | uspto-grants-2013_02 |
| ORD ID | ord-85b7039681764b56b930fd22abf2fe66 |
| 出典メモ | uspto-grants-2013_02 |