反応式
[CH2:1]([N:8]1[C:14](=[O:15])[C@H:13]2[CH2:16][CH2:17][CH2:18][C@H:12]2[NH:11][C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]1=2)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:23][CH2:24][C:25](Cl)=[O:26]>ClCCCl>[CH2:1]([N:8]1[C:14](=[O:15])[C@H:13]2[CH2:16][CH2:17][CH2:18][C@H:12]2[N:11]([C:25](=[O:26])[CH2:24][Cl:23])[C:10]2[CH:19]=[CH:20][CH:21]=[CH:22][C:9]1=2)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1参加物
4
反応物 2
生成物 1
試薬・触媒・溶媒 1
実験手順
On a water-bath kept at 14° C., to a solution of (3aR*,10aS*)-9-benzyl-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (5.85 g, 20 mmol) in 1,2-dichloroethane (20 mL) was added dropwise a solution of chloroacetyl chloride (2.5 g, 22 mmol) in 1,2-dichloroethane (15 mL), and the mixture was stirred for 10 minutes. The aqueous layer of this mixture was separated, and the organic layer was washed with water and a saturated aqueous solution of sodium chloride, dried over magnesium sulfate, which was subjected to filtration, and the filtrate was concentrated under reduced pressure. The concentrate was recrystallized from dichloromethane-hexane to give 6.49 g (yield 88%) of the titled compound, m.p. 154°-156° C.
後処理
- customThe aqueous layer of this mixture was separated
- washthe organic layer was washed with water
- dry with materiala saturated aqueous solution of sodium chloride, dried over magnesium sulfate, which
- filtrationwas subjected to filtration
- concentrationthe filtrate was concentrated under reduced pressure
- customThe concentrate was recrystallized from dichloromethane-hexane
出典と根拠
- ORDレコード
- ord-ff6fcf84233f492ebcd5935e0b4a2bcf
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05834463
関連ノート
読み込み中…