Ammonia → 3-Benzyl-1,2,4-thiadiazol-5-amine
反応式
[CH2:1]([C:8]1[N:12]=[C:11](Cl)[S:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH3:14]>>[CH2:1]([C:8]1[N:12]=[C:11]([NH2:14])[S:10][N:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1参加物
3
反応条件
- 温度
- 50 °C
実験手順
A mixture of 3-benzyl-5-chloro-[1,2,4]thiadiazole (105 mg, 0.5 mmol) in ammonia (2 N in MeOH, 2 ml) was heated in a pressure tube at 50° C. for 5 h. The solvents were evaporated, the residue diluted with dichloromethane, the white solid (ammonium chloride) was filtered off, the filtrate was concentrated and then purified by silica gel chromatography using dichloromethane/methanol as eluent. The title compound was obtained as a light yellow liquid (40 mg, 41%). MS ISP (m/e): 192.1 (100) [(M+H)+].
後処理
- customThe solvents were evaporated
- additionthe residue diluted with dichloromethane
- filtrationthe white solid (ammonium chloride) was filtered off
- concentrationthe filtrate was concentrated
- custompurified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-627c223dfef649a5a6faf340263f78f3
- 出典データセット
- uspto-grants-2012_10
- 特許番号
- US08288403B2
反応ノート
読み込み中…