Sodium borohydride → HCID 22563217、化合物
反応式
[Cl:1][CH2:2][C:3]([C:5]1[N:10]=[CH:9][CH:8]=[CH:7][N:6]=1)=[O:4].[BH4-].[Na+]>C(O)C>[Cl:1][CH2:2][CH:3]([C:5]1[N:10]=[CH:9][CH:8]=[CH:7][N:6]=1)[OH:4]参加物
4
実験手順
2-Chloro-1-pyrimidin-2-ylethanone (6.15 g, 39.3 mmol) was dissolved in ethanol (125 ml) and CeCl3.7H2O (14.64 g, 39.3 mmol) was added. Stirring was continued for 10 min then sodium borohydride (1.49 g, 39.3 mmol) was added over 2 min. After 1 hr the solid was filtered and the filtrate evaporated. Sat. ammonium chloride solution (25 ml) was added followed by brine (250 ml) and the mixture adjusted to pH3-4 with 1N.HCl. Extraction with ethyl acetate (3×250 ml) afforded an amber oil which was chromatographed over silica gel (150 g) to give the product as a pale yellow oil (3.85 g)
後処理
- filtrationAfter 1 hr the solid was filtered
- customthe filtrate evaporated
- additionSat. ammonium chloride solution (25 ml) was added
- extractionExtraction with ethyl acetate (3×250 ml)
- customafforded an amber oil which
- customwas chromatographed over silica gel (150 g)
出典と根拠
- ORDレコード
- ord-acbe899ca66e40dbb461152de1c95f69
- 出典データセット
- uspto-grants-2005_03
- 特許番号
- US06861438B2
反応ノート
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