Isopropyl iodide → 7-[4-(4-Chlorobenzoyl)benzyl]-1-isopropyl-3-methylxanthine

HRID 1291412

反応式

HRID 1291412 の反応式
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH2:11][C:12]3[CH:17]=[CH:16][C:15]([C:18](=[O:26])[C:19]4[CH:24]=[CH:23][C:22]([Cl:25])=[CH:21][CH:20]=4)=[CH:14][CH:13]=3)[C:6]=2[C:5](=[O:27])[NH:4][C:3]1=[O:28].C(=O)([O-])[O-].[K+].[K+].[CH:35](I)([CH3:37])[CH3:36]>CN(C=O)C.O>[Cl:25][C:22]1[CH:23]=[CH:24][C:19]([C:18]([C:15]2[CH:14]=[CH:13][C:12]([CH2:11][N:7]3[C:6]4[C:5](=[O:27])[N:4]([CH:35]([CH3:37])[CH3:36])[C:3](=[O:28])[N:2]([CH3:1])[C:10]=4[N:9]=[CH:8]3)=[CH:17][CH:16]=2)=[O:26])=[CH:20][CH:21]=1

参加物

6

反応物 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 189188013-Methyl-7-[4-(4-chlorobenzoyl)benzyl]xanthine

生成物 1

HCID 189192457-[4-(4-Chlorobenzoyl)benzyl]-1-isopropyl-3-methylxanthine収率 6.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3-methyl-7-[4-(4-chlorobenzoyl)-benzyl]xanthine (544 mg), potassium carbonate (202 mg) and isopropyl iodide (356 mg) in DMF (10 ml) was stirred at 60° C. for 5 hours. This reaction mixture was poured in water and extracted with ethyl acetate. The extract was washed with water, dried and concentrated. The residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1) and recrystallized from acetone-hexane to provide the title compound as colorless solid (38 mg).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1)
  6. customrecrystallized from acetone-hexane

出典と根拠

ORDレコード
ord-bcf7b3611c324a34a886238f54b510c8
出典データセット
uspto-grants-1998_05
特許番号
US05753664

関連ノート

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