反応式
[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][C:5]#[N:6].N[NH:9][C:10]([NH2:12])=[S:11].C(=O)([O-])[O-].[K+].[K+]>FC(F)(F)C(O)=O.O>[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][C:5]1[S:11][C:10]([NH2:12])=[N:9][N:6]=1参加物
6
実験手順
A solution of 2.00 ml (17.7 mmol) of 3-(dimethylamino)propanenitrile and 1.70 g (18.6 mmol) of thiosemicarbazide in trifluoroacetic acid (5 ml) was heated at 80° C. for 6 hr. The reaction solution was cooled to room temperature and was then diluted with water. The diluted solution was rendered weakly basic by the addition of a 10% aqueous potassium carbonate solution. The solution was extracted with chloroform, and the extract was dried over anhydrous sodium sulfate. The filtrate was concentrated, and the residue was washed with diethyl ether-ethyl acetate to give 1.00 g (yield 33%) of the title compound.
後処理
- extractionThe solution was extracted with chloroform
- dry with materialthe extract was dried over anhydrous sodium sulfate
- concentrationThe filtrate was concentrated
- washthe residue was washed with diethyl ether-ethyl acetate
出典と根拠
- ORDレコード
- ord-f84e073f8f244555808346b823bba7e4
- 出典データセット
- uspto-grants-2011_02
- 特許番号
- US07879808B2
関連ノート
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