Triethylamine → HCID 20299638、化合物
反応式
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[N:6]([CH:8]=[CH:9][N:10]=2)[CH:7]=1.C(N(CC)CC)C.[F:18][C:19]([F:23])([F:22])[S:20]Cl>C(#N)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[N:6]([C:8]([S:20][C:19]([F:23])([F:22])[F:18])=[CH:9][N:10]=2)[CH:7]=1参加物
5
実験手順
A solution of 6-chloroimidazo[1,2-a]pyrazine (3.07 g, 0.020 mol) in acetonitrile (50 ml) containing 1.01 g (0.010 mol) of triethylamine is treated with a stream of trifluoromethanesulfenyl chloride gas at 25° C. under nitrogen. After 1 hour the solution is flushed with nitrogen, concentrated under vacuum, and the residue partitioned between water-chloroform. The chloroform extract is dried over sodium sulfate, filtered and concentrated under vacuum to give crude 6-chloro-3-trifluoromethylthioimidazo[1,2-a]pyrazine which is purified by fractional sublimation.
後処理
- customAfter 1 hour the solution is flushed with nitrogen
- concentrationconcentrated under vacuum
- customthe residue partitioned between water-chloroform
- extractionThe chloroform extract
- dry with materialis dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated under vacuum
出典と根拠
- ORDレコード
- ord-c1e3167853d0466cac8fceef002d7bf9
- 出典データセット
- uspto-grants-1980_12
- 特許番号
- US04242344
反応ノート
読み込み中…