Formamide → HCID 178484998、化合物
反応式
[C:1]([NH:3][C:4]([NH:7][CH2:8][CH2:9][S:10][CH2:11][C:12](=O)[CH:13]([NH:15][CH:16]=O)[CH3:14])=[N:5][CH3:6])#[N:2].C([O-])=O.[NH4+].C([O-])([O-])OC.O.O.O.O.P([O-])([O-])(O)=O.[NH4+].[Na+].C([NH2:41])=O>>[C:1]([NH:3][C:4]([NH:5][CH3:6])=[N:7][CH2:8][CH2:9][S:10][CH2:11][C:12]1[N:41]=[CH:16][NH:15][C:13]=1[CH3:14])#[N:2]参加物
6
反応条件
- 温度
- 100 °C
実験手順
To 136 mg of N-cyano-N'-[2-(3-formylamino-2-oxobutylthio)ethyl]-N"-methylguanidine, 320 mg of amonium formate, 0.6 ml of methyl orthoformate and 209 mg of sodium ammonium hydrogenphosphate tetrahydrate was added 2.5 ml of formamide, and the mixture was stirred at 100° C. for 2 hours. The reaction mixture was cooled and insoluble substances were removed, and the solvent was removed under reduced pressure and the obtained residue was refined by silica gel column chromatography (eluting solvent: chloroform/ethanol=5/1) and recrystallized from isopropanol/ether (60/40) to obtain 100 mg of intended Cimetidine (the yield was 87%).
後処理
- temperatureThe reaction mixture was cooled
- custominsoluble substances were removed
- customthe solvent was removed under reduced pressure
- washthe obtained residue was refined by silica gel column chromatography (eluting solvent: chloroform/ethanol=5/1)
- customrecrystallized from isopropanol/ether (60/40)
出典と根拠
- ORDレコード
- ord-d8c756f6edd649dda9bd58fd304200f5
- 出典データセット
- uspto-grants-1989_12
- 特許番号
- US04886910
反応ノート
読み込み中…