Sodium Iodide → HCID 17830871、化合物

HRID 1249988ノート

反応式

HRID 1249988 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[C:13]3[CH:18]=[CH:17][C:16]([NH2:19])=[CH:15][C:14]=3[O:20][CH3:21])[CH2:10][CH2:9][CH2:8][CH:7]([CH2:23][C:24]([O:26][CH3:27])=[O:25])[C:6]=2[CH:28]=1.C(=O)([O-])[O-].[Na+].[Na+].[Br-].[Br-].[C:37]1([CH3:44])[C:38]([CH3:43])=[CH:39][CH:40]=[CH:41][CH:42]=1.[I-].[Na+]>C(O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([C:12](=[O:22])[C:13]3[CH:18]=[CH:17][C:16]([N:19]4[CH2:43][C:38]5[C:37](=[CH:42][CH:41]=[CH:40][CH:39]=5)[CH2:44]4)=[CH:15][C:14]=3[O:20][CH3:21])[CH2:10][CH2:9][CH2:8][CH:7]([CH2:23][C:24]([O:26][CH3:27])=[O:25])[C:6]=2[CH:28]=1

参加物

6

反応物 4

HCID 5238Sodium IodideHCID 10340Sodium CarbonateHCID 18001039HCID 18001039、化合物HCID 22258337HCID 22258337、化合物

生成物 1

HCID 17830871HCID 17830871、化合物収率 9.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
65 °C

実験手順

To a suspension of 7-chloro-5-methoxycarbonylmethyl-1-(2-methoxy-4-aminobenzoyl)-2,3,4,5-tetrahydro-1H-benzazepine (2.6 g) in ethanol (100 ml) are added sodium carbonate (1.5 g), o-xylene dibromide (1.87 g) and sodium iodide (2.42 g), and the mixture is stirred at 60-70° C. for three hours. The mixture is evaporate to remove the solvent, and to the residue is added water, and the mixture is extracted with ethyl acetate. The extract is dried, and evaporate to remove the solvent. The residue is purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:10→1:5) to give 7-chloro-5-methoxycarbonylmethyl-1-[2-methoxy-4-(2-isoindolinyl)benzoyl]-2,3,4,5-tetrahydro-1H-benzazepine (0.32 g) as colorless amorphous.

後処理

  1. customThe mixture is evaporate
  2. customto remove the solvent
  3. additionto the residue is added water
  4. extractionthe mixture is extracted with ethyl acetate
  5. customThe extract is dried
  6. customevaporate
  7. customto remove the solvent
  8. customThe residue is purified by silica gel column chromatography (solvent; ethyl acetate:n-hexane=1:10→1:5)

出典と根拠

ORDレコード
ord-6e67d07539204826931359aa4614729c
出典データセット
uspto-grants-2002_01
特許番号
US06335327B1

反応ノート

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