Methyl isothiocyanate → N-Methyl-N'-[2-[[3-(N,N-dimethylaminomethyl)phenyl]methylthio]ethyl]thiourea
反応式
[CH3:1][N:2]([CH2:4][C:5]1[CH:6]=[C:7]([CH2:11][S:12][CH2:13][CH2:14][NH2:15])[CH:8]=[CH:9][CH:10]=1)[CH3:3].[CH3:16][N:17]=[C:18]=[S:19]>C(#N)C>[CH3:16][NH:17][C:18]([NH:15][CH2:14][CH2:13][S:12][CH2:11][C:7]1[CH:8]=[CH:9][CH:10]=[C:5]([CH2:4][N:2]([CH3:1])[CH3:3])[CH:6]=1)=[S:19]参加物
4
実験手順
2-[[3-(N,N-Dimethylaminomethyl)phenyl]methylthio]ethanamine (5 g) and methyl isothiocyanate (1.62 g) were stirred at room temperature in acetonitrile for 18 hours. The solvent was removed and the residue was column chromatographed on silica using a mixture of ethyl acetate and methanol as eluent to give the title compound as a pale yellow oil. TLC silica; ethyl acetate:isopropanol:water:0.88 ammonia (25:15:8:2) Rf 0.61.
後処理
- customThe solvent was removed
- customchromatographed on silica using
- additiona mixture of ethyl acetate and methanol as eluent
出典と根拠
- ORDレコード
- ord-04f5ef278ce147c68455c782963f3a1d
- 出典データセット
- uspto-grants-1991_06
- 特許番号
- US05021429
反応ノート
読み込み中…