(2-Bromo-4-methylthiazol-5-yl)methanol → 2-Bromo-4-methylthiazole-5-carbaldehyde
反応式
[Br:1][C:2]1[S:3][C:4]([CH2:8][OH:9])=[C:5]([CH3:7])[N:6]=1>C(Cl)(Cl)Cl.O=[Mn]=O>[Br:1][C:2]1[S:3][C:4]([CH:8]=[O:9])=[C:5]([CH3:7])[N:6]=1参加物
4
実験手順
A mixture of (2-bromo-4-methylthiazol-5-yl)methanol of preparation 97 (3.8 g, 18.4 mmol) and MnO2 (16.5 g, 0.18 mmol) in CHCl3 (180 mL) was stirred at room temperature overnight. TLC (petroleum ether/EtOAc=3:1) showed the reaction was complete. The reaction mixture was filtered and the filtrate was concentrated in vacuum. The residue was purified by a Biotage silica gel cartridge (EA/PE=30%, Rf=0.5) to give the title compound as a white solid (1.8 g, 47%) as a white solid, and as well as impure 2-bromo-4-methylthiazole-5-carbaldehyde (1.3 g, 34%) as an off-white solid.
後処理
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated in vacuum
- customThe residue was purified by a Biotage silica gel cartridge (EA/PE=30%, Rf=0.5)
出典と根拠
- ORDレコード
- ord-a65df0c0dffe41ff9de7d8a993b7d831
- 出典データセット
- uspto-grants-2014_12
- 特許番号
- US08916593B2
反応ノート
読み込み中…