Sodium Bicarbonate → HCID 22563232、化合物
反応式
[Cl:1][CH:2]=[C:3]([C:15]1[N:20]=[CH:19][CH:18]=[CH:17][N:16]=1)[O:4][Si](C(C)C)(C(C)C)C(C)C.C(=O)(O)[O-].[Na+]>C(#N)C>[Cl:1][CH2:2][C:3]([C:15]1[N:20]=[CH:19][CH:18]=[CH:17][N:16]=1)=[O:4]参加物
4
実験手順
2-{2-Chloro-1-[(triisopropylsilyl)oxy]ethenyl}pyrimidine (19.4 g, 62.2 mmol) was dissolved in acetonitrile (90 ml) and treated with 48% HF (10 ml) for 4 hr. Sat. sodium bicarbonate solution (ca. 250 ml) was then added carefully to pH7 and the mixture extracted with CH2Cl2 (3×200 ml). After drying (Na2SO4), filtration and evaporation two oils were obtained, the upper colorless oil was decanted off and discarded and the lower oil crystallized to an oily solid. Chromatography over silica gel (500 g) eluting with 2.5% MeOH—CHCl3 gave the product as a pale yellow solid (6.50 g) mp:73-80°.
後処理
- additiontreated with 48% HF (10 ml) for 4 hr
- extractionthe mixture extracted with CH2Cl2 (3×200 ml)
- customAfter drying
- filtration(Na2SO4), filtration
- customevaporation two oils
- customwere obtained
- customthe upper colorless oil was decanted off
- customthe lower oil crystallized to an oily solid
- washChromatography over silica gel (500 g) eluting with 2.5% MeOH—CHCl3
出典と根拠
- ORDレコード
- ord-d227cdd31f984490823d8912c16e0144
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06852731B2
反応ノート
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