反応式
[CH:1]([C:4]1([CH3:23])[C:8](=[O:9])[NH:7][C:6]([C:10]2[N:15]=[C:14]3[CH:16]=[CH:17][O:18][C:13]3=[CH:12][C:11]=2[C:19]([O:21][CH3:22])=[O:20])=[N:5]1)([CH3:3])[CH3:2].Cl.C([BH3-])#N.[Na+].[OH-].[Na+]>CO.CN(C1C=CC(N=NC2C=CC(S(O)(=O)=O)=CC=2)=CC=1)C>[CH:1]([C:4]1([CH3:23])[C:8](=[O:9])[NH:7][CH:6]([C:10]2[N:15]=[C:14]3[CH:16]=[CH:17][O:18][C:13]3=[CH:12][C:11]=2[C:19]([O:21][CH3:22])=[O:20])[NH:5]1)([CH3:3])[CH3:2]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 0 °C
実験手順
A solution of 22.1 mmol of methyl 5-(4-isopropyl-4-methyl-5-oxo-2-imidazolin-2-yl)furo[3,2-b]pyridine-6-carboxylate in methanol is cooled to 0° C. and a few drops of methyl orange indicator added. The solution is stirred and treated with 22.1 mmol of concentrated hydrochloric acid. The solution is then treated with 22.1 mmol of sodium cyanoborohydride, and the pH maintained at ~3 by the additon of 2N methanolic HCl, stirred overnight, cooled to 0° C. and the pH of the solution adjusted to about 0 with HCl to decompose residual NaCNBH3. The pH is thereafter adjusted to 5-6 with 5N NaOH. The methanol is removed in vacuo and water added to dissolve inorganic salts. The mixture is extracted with CH2Cl2 and the extracts dried and concentrated to give the title compound.
後処理
- stirringstirred overnight
- customThe methanol is removed in vacuo and water
- additionadded
- dissolutionto dissolve inorganic salts
- extractionThe mixture is extracted with CH2Cl2
- customthe extracts dried
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-8ce18af375ba448b866c5002650a39d8
- 出典データセット
- uspto-grants-1986_08
- 特許番号
- US04608079
関連ノート
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