Phosphorus oxychloride → 4-Chloro-2-ethylthieno(3,2-d)pyrimidine
反応式
[CH2:1]([C:3]1[N:4]=[C:5](O)[C:6]2[S:11][CH:10]=[CH:9][C:7]=2[N:8]=1)[CH3:2].P(Cl)(Cl)([Cl:15])=O>>[Cl:15][C:5]1[C:6]2[S:11][CH:10]=[CH:9][C:7]=2[N:8]=[C:3]([CH2:1][CH3:2])[N:4]=1参加物
3
実験手順
2-Ethyl-4-hydroxythieno[3,2-d]pyrimidine (0.6725 g, 0.00373M) was refluxed with phosphorus oxychloride (20 ml) for 2 hours. The reaction mixture was cooled, concentrated under vacuum, the residue dissolved in methylene chloride, poured over ice and water and basified with ammonia. The layers were separated and the aqueous layer extracted with ether. The combined organic extracts were washed with brine, dried (MgSO4) and concentrated under vacuum to obtain the product, 0.65 g, as a tan solid, m.p. 46°-48° C. the structure of which was confirmed by NMR.
後処理
- temperatureThe reaction mixture was cooled
- concentrationconcentrated under vacuum
- dissolutionthe residue dissolved in methylene chloride
- additionpoured over ice and water and basified with ammonia
- customThe layers were separated
- extractionthe aqueous layer extracted with ether
- washThe combined organic extracts were washed with brine
- dry with materialdried (MgSO4)
- concentrationconcentrated under vacuum
- customto obtain the product, 0.65 g
出典と根拠
- ORDレコード
- ord-586c38cf10a64d378fa2584155ead93b
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04889856
反応ノート
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