2,4-Dibromo-thiazole-5-carbaldehyde → 2,4-Dibromothiazole-5-methanol
反応式
[Br:1][C:2]1[S:3][C:4]([CH:8]=[O:9])=[C:5]([Br:7])[N:6]=1.[BH4-].[Na+]>CO>[Br:1][C:2]1[S:3][C:4]([CH2:8][OH:9])=[C:5]([Br:7])[N:6]=1参加物
4
実験手順
2,4-Dibromo-thiazole-5-carbaldehyde (2.0 g, 7.4 mmol) in methanol (80 mL) was treated with NaBH4 (419 mg, 11.0 mmol). The reaction mixture was stirred at rt overnight, quenched with 10% NaOH, diluted with water and extracted with ethyl acetate (2×). The solvent was removed, and the resulting residue was chromatographed using hexane/ethyl acetate (3:1) to give the title compound (1.84 g, 91%). MS (DCI/NH3) m/z 274 (M)+. 1H NMR (500 MHz, CDCl3) δ ppm 2.11 (s, 1H) 4.78 (s, 2H).
後処理
- customquenched with 10% NaOH
- additiondiluted with water
- extractionextracted with ethyl acetate (2×)
- customThe solvent was removed
- customthe resulting residue was chromatographed
出典と根拠
- ORDレコード
- ord-7ac8d0d874d84bbda6bc028bddfb0286
- 出典データセット
- uspto-grants-2010_04
- 特許番号
- US07704997B1
反応ノート
読み込み中…