2-(2-Amino-1,3-thiazol-4-yl)acetamide → 4-Thiazoleacetonitrile, 2-amino-
反応式
[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH2:7][C:8]([NH2:10])=O)[N:6]=1>P(Cl)(Cl)(Cl)=O>[NH2:1][C:2]1[S:3][CH:4]=[C:5]([CH2:7][C:8]#[N:10])[N:6]=1参加物
3
反応条件
- 温度
- 90 °C
実験手順
A mixture of the product from step (i) (9.5 g) and phosphorous oxychloride (30 ml) was heated at 90° C. for 2 hours. The mixture was evaporated under reduced pressure and poured onto a mixture of ice water and ethyl acetate. The aqueous phase was adjusted to pH 9 with sodium bicarbonate and extracted repeatedly with ethyl acetate. The combined extract was dried (MgSO4) and evaporated. The residue was purified by chromatography eluting with ethyl acetate. Yield 6.1 g. 1H NMR: δ (DMSO) 7.08(br s,2H), 6.40(s,1H), 3.77(s,2H).
後処理
- customThe mixture was evaporated under reduced pressure
- additionpoured onto a mixture of ice water and ethyl acetate
- extractionextracted repeatedly with ethyl acetate
- extractionThe combined extract
- dry with materialwas dried (MgSO4)
- customevaporated
- customThe residue was purified by chromatography
- washeluting with ethyl acetate
出典と根拠
- ORDレコード
- ord-d0ad4b5a45564d7898a3883e7bdd7a32
- 出典データセット
- uspto-grants-2000_08
- 特許番号
- US06107297
反応ノート
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