Hydrochloric Acid → 1,4-Diazepan-5-one--hydrogen chloride (1/1)
反応式
[ClH:1].C([N:9]1[CH2:15][CH2:14][C:13](=[O:16])[NH:12][CH2:11][CH2:10]1)C1C=CC=CC=1.[H][H]>C(O)C.CO.[C].[Pd]>[ClH:1].[NH:9]1[CH2:15][CH2:14][C:13](=[O:16])[NH:12][CH2:11][CH2:10]1参加物
7
実験手順
1M HCl in ethanol (7.2 mL) and 10% palladium-carbon (0.34 g) were added to 1-benzylhexahydro-1H-1,4-diazepin-5-one (1.490 g) in methanol (10 mL) at room temperature, and the resultant mixture was stirred in a hydrogen atmosphere for 4 hours. After the reaction atmosphere was purged with nitrogen, insoluble matter was removed by filtration. The solvent of the filtrate was evaporated under reduced pressure, and diethyl ether was added to the residue, and then the precipitated solid was recovered by filtration, to thereby give the title compound (1.045 g, 96%).
後処理
- customAfter the reaction atmosphere
- customwas purged with nitrogen, insoluble matter
- customwas removed by filtration
- customThe solvent of the filtrate was evaporated under reduced pressure, and diethyl ether
- additionwas added to the residue
- filtrationthe precipitated solid was recovered by filtration
出典と根拠
- ORDレコード
- ord-fa7de088fada47f69ce40bd3dfec0682
- 出典データセット
- uspto-grants-2009_11
- 特許番号
- US07622471B2
反応ノート
読み込み中…