反応式
[NH2:1][C@H:2]([C:7]([OH:9])=[O:8])[CH2:3][CH2:4]ON.CS/[C:12](/[NH2:15])=[N:13]/[NH2:14].I.[N:17]#[N:18].Cl>[OH-].[Na+]>[NH2:1][CH:2]([CH2:3][CH2:4][NH:14][NH:13][CH:12]=[N:15][NH:17][NH2:18])[C:7]([OH:9])=[O:8]参加物
6
反応条件
- 温度
- 4 °C
実験手順
Mix canaline (2.65 g, 20 mmol) and S-methylisothiosemicarbazide hydroiodide (4.66 g, 20 mmol) in 1M NaOH (40 ml) and stir under a blanket N2 at 40° C. for 48 hours. Neutralize the reaction with 1M HCl and blow to a residue with a stream of N2. Apply the residue to a Dowex AG50-X8 column and elute with 0.2M NH4OH. Lyophilize the fractions containing the desired product and take up the resulting solid in water (20 ml). Add flavianic acid (3.2 g) in water (20 ml) and cool the solution to 4° C. for 16 hours. Filter the resulting solid and crystallize to yield the title compound.
後処理
- washApply the residue to a Dowex AG50-X8 column and elute with 0.2M NH4OH
- additioncontaining the desired product
- filtrationFilter the resulting solid
- customcrystallize
出典と根拠
- ORDレコード
- ord-c8cda447d7c7482da4b25906b25fe5f4
- 出典データセット
- uspto-grants-1994_06
- 特許番号
- US05318992
関連ノート
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