Thionyl Chloride → HCID 22349860、化合物
反応式
[C:1]([C:5]1[N:10]=[C:9](O)[CH:8]=[C:7]([CH:12]([F:14])[F:13])[N:6]=1)([CH3:4])([CH3:3])[CH3:2].S(Cl)([Cl:17])=O.C(=O)(O)[O-].[Na+]>ClCCl>[C:1]([C:5]1[N:10]=[C:9]([Cl:17])[CH:8]=[C:7]([CH:12]([F:14])[F:13])[N:6]=1)([CH3:4])([CH3:3])[CH3:2]参加物
5
実験手順
2.8 g of 2-tert-butyl-4-hydroxy-6-difluoromethyl-pyrimidine (13.9 mmol) and 3 ml of thionylchloride were stirred 14 h at room temperature and an additional 3 h at 76° C. 20 ml of dichloromethane were added with cooling, followed by addition of 15 ml of a saturated aqueous solution of sodium bicarbonate. The organic layer was separated, dried over magnesium sulfate and the solvent was evaporated to yield the crude title compound which was purified by column chromatography on silica gel (dichloromethane/hexane 1:1) to yield 0.8 g of product.
後処理
- temperaturewith cooling
- customThe organic layer was separated
- dry with materialdried over magnesium sulfate
- customthe solvent was evaporated
- customto yield the crude title compound which
- customwas purified by column chromatography on silica gel (dichloromethane/hexane 1:1)
出典と根拠
- ORDレコード
- ord-01d7a881801c46818be5878901fd579e
- 出典データセット
- uspto-grants-2005_07
- 特許番号
- US06919342B2
反応ノート
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