Potassium Carbonate → 7-[4-(4-Chlorobenzoyl)benzyl]-3-methyl-1-propylxanthine

HRID 1291410

反応式

HRID 1291410 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+].[CH2:35](I)[CH2:36][CH3:37]>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]([CH2:35][CH2:36][CH3:37])[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 11430Potassium CarbonateHCID 336431-IodopropaneHCID 189188013-Methyl-7-[4-(4-chlorobenzoyl)benzyl]xanthine

生成物 1

HCID 189190077-[4-(4-Chlorobenzoyl)benzyl]-3-methyl-1-propylxanthine収率 48.4%

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 (657 mg), potassium carbonate (242 mg) and propyl iodide (427 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 ethyl acetate to provide the title compound as colorless solid (352 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 ethyl acetate

出典と根拠

ORDレコード
ord-4988ba6bbf1e484989f3db1b12a121fc
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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