反応式
[CH3:1][N:2]([CH3:16])[CH2:3][CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:14]#[N:15])[CH:12]=2)[NH:7][CH:6]=1.C(N(CC)CC)C.[SH2:24]>CN(C)C=O>[CH3:16][N:2]([CH3:1])[CH2:3][CH2:4][C:5]1[C:13]2[C:8](=[CH:9][CH:10]=[C:11]([C:14](=[S:24])[NH2:15])[CH:12]=2)[NH:7][CH:6]=1参加物
5
実験手順
A solution of 3-[2-(dimethylamino)ethyl]-1H-indole-5-carbonitrile (13.0 g) and triethylamine (50 ml) in dimethylformamide (300 ml) was stirred for 2 h whilst gaseous hydrogen sulphide was bubbled through it. More triethylamine (10 ml) was added and the solution was stirred at room temperature for 2 days, then evaporated in vacuo to give an oil (15 g) which was partitioned between ethyl acetate (500 ml) and water (3×250 ml). The organic layer was dried (MgSO4) pre-absorbed onto silica and purified by flash chromatography (A). The appropriate fractions were combined, concentrated in vacuo and triturated with ether (250 ml) to give the title compound (12.0 g) as a solid, m.p. 155°.
後処理
- customwas bubbled through it
- additionMore triethylamine (10 ml) was added
- customevaporated in vacuo
出典と根拠
- ORDレコード
- ord-2faf13d4fbc9489b9d679b30d03af470
- 出典データセット
- uspto-grants-1989_05
- 特許番号
- US04833153
関連ノート
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