反応式
[C:1]1(=[O:29])[N:5]([CH2:6][C:7]([N:9]2[CH:15]3[CH2:16][CH2:17][CH2:18][CH:14]3[C:13](=[O:19])[NH:12][C:11]3[CH:20]=[CH:21][CH:22]=[CH:23][C:10]2=3)=[O:8])[C:4](=[O:24])[C:3]2=[CH:25][CH:26]=[CH:27][CH:28]=[C:2]12.C(=O)([O-])[O-].[K+].[K+].C(Cl)(Cl)Cl>BrC1C=CC=CC=1.[Cu]I>[C:2]1([N:12]2[C:13](=[O:19])[CH:14]3[CH2:18][CH2:17][CH2:16][CH:15]3[N:9]([C:7](=[O:8])[CH2:6][N:5]3[C:4](=[O:24])[C:3]4=[CH:25][CH:26]=[CH:27][CH:28]=[C:2]4[C:1]3=[O:29])[C:10]3[CH:23]=[CH:22][CH:21]=[CH:20][C:11]2=3)[CH:3]=[CH:25][CH:26]=[CH:27][CH:28]=1参加物
6
反応物 3
生成物 1
試薬・触媒・溶媒 2
実験手順
To a suspension of 4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (584 mg, 1.5 mmol) and potassium carbonate (228 mg, 1.6 mmol) in bromobenzene (3 mL) was added copper (I) iodide (57 mg, 0.3 mmol), and the mixture was heated for 90 minutes under reflux. To the reaction mixture was added chloroform, which was subjected to filtration, and the filtrate was concentrated under reduced pressure. The concentrate was recrystallized from chloroform-ethanol-hexane to give 440 mg (yield 63%) of a mixture of cis-compound and trans-compound (3:2), m.p. 272°-273° C.
後処理
- temperaturethe mixture was heated for 90 minutes
- temperatureunder reflux
- filtrationwas subjected to filtration
- concentrationthe filtrate was concentrated under reduced pressure
- customThe concentrate was recrystallized from chloroform-ethanol-hexane
出典と根拠
- ORDレコード
- ord-497a574e32204599bf338740bc3a80f7
- 出典データセット
- uspto-grants-1998_11
- 特許番号
- US05834463
関連ノート
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