Ammonium cerium (IV) nitrate → HCID 70111246、化合物

HRID 356161

反応式

HRID 356161 の反応式
C[O:2][C:3]1[C:38]([CH3:39])=[C:37]([CH3:40])[C:36]([O:41]C)=[C:35]([CH3:43])[C:4]=1[CH2:5][N:6]1[C:12](=[O:13])[C@H:11]2[CH2:14][CH2:15][CH2:16][C@H:10]2[N:9]([C:17](=[O:30])[CH2:18][N:19]2[C:23](=[O:24])[C:22]3=[CH:25][CH:26]=[CH:27][CH:28]=[C:21]3[C:20]2=[O:29])[C:8]2[CH:31]=[CH:32][CH:33]=[CH:34][C:7]1=2.[N+]([O-])([O-])=O.[Ce+4].[NH4+].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>C(#N)C.O>[C:20]1(=[O:29])[N:19]([CH2:18][C:17]([N:9]2[C@@H:10]3[CH2:16][CH2:15][CH2:14][C@@H:11]3[C:12](=[O:13])[N:6]([CH2:5][C:4]3[C:3](=[O:2])[C:38]([CH3:39])=[C:37]([CH3:40])[C:36](=[O:41])[C:35]=3[CH3:43])[C:7]3[CH:34]=[CH:33][CH:32]=[CH:31][C:8]2=3)=[O:30])[C:23](=[O:24])[C:22]2=[CH:25][CH:26]=[CH:27][CH:28]=[C:21]12

参加物

5

反応物 2

HCID 9869224Ammonium cerium (IV) nitrateHCID 86753321HCID 86753321、化合物

生成物 1

HCID 70111246HCID 70111246、化合物収率 63.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒3 回HCID 6342Acetonitrile溶媒2 回

実験手順

In a mixture of acetonitrile (3 mL) and water (2 mL) was suspended (3aR*,10aS*)-9-(2,5-dimethoxy-3,4,6-trimethylbenzyl)-4-(phthalimidoacetyl)-2,3,3a,4,9,10a-hexahydrobenzo[b]cyclopenta[e][1,4]diazepin-10(1H)-one (0.5 g, 0.86 mmol). To the suspension was added, while stirring, a solution of ammonium cerium (IV) nitrate (1.4 g, 2.55 mmol) in a mixture of acetonitrile (2 mL) and water (2 mL). The reaction mixture was stirred for one hour, which was diluted with water, followed by extraction with chloroform. The extract was washed with water and dried, then the solvent was distilled off. The residue was crystallized from ethyl acetate to give 300 mg (yield 63%) of the titled compound, m.p. 258°-260° C.

後処理

  1. additionTo the suspension was added
  2. stirringThe reaction mixture was stirred for one hour
  3. extractionfollowed by extraction with chloroform
  4. washThe extract was washed with water
  5. customdried
  6. distillationthe solvent was distilled off
  7. customThe residue was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-847abb0f88834618ac59ca324403a869
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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