Ammonia → 2-(Methylthio)pyrimidin-4-amine
反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH3:9])[N:3]=1.[NH3:10]>CO>[CH3:9][S:8][C:4]1[N:3]=[C:2]([NH2:10])[CH:7]=[CH:6][N:5]=1参加物
4
実験手順
A mixture of 4-chloro-2-methylsulfanylpyrimidine (8 g) and 7N ammonia in methanol (100 mL) at 100° C. was stirred for 2 days in a sealed tube, cooled, concentrated, treated with water, and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The concentrate was triturated with ethyl ether and filtered. 1H NMR (300 MHz, CDCl3) δ 8.06 (d, 1H), 6.12 (d, 1H), 4.83 (s, 2H), 2.51 (s, 3H).
後処理
- temperaturecooled
- concentrationconcentrated
- additiontreated with water
- extractionextracted with ethyl acetate
- washThe extract was washed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe concentrate was triturated with ethyl ether
- filtrationfiltered
出典と根拠
- ORDレコード
- ord-ee4c67b25ee64efdb3c0893c80b0defa
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07737159B2
反応ノート
読み込み中…