Benzyl Chloride → 7-Benzyl-3-methylxanthine

HRID 1995

反応式

HRID 1995 の反応式
[H-].[Na+].[CH3:3][N:4]1[C:12]2[N:11]=[CH:10][NH:9][C:8]=2[C:7](=[O:13])[NH:6][C:5]1=[O:14].[H][H].[CH2:17](Cl)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>CN(C)C=O.O>[CH2:17]([N:9]1[C:8]2[C:7](=[O:13])[NH:6][C:5](=[O:14])[N:4]([CH3:3])[C:12]=2[N:11]=[CH:10]1)[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

参加物

7

反応物 4

HCID 7503Benzyl ChlorideHCID 24758Sodium hydrideHCID 706393-MethylxanthineHCID 178418361HCID 178418361、化合物

生成物 1

HCID 6856307-Benzyl-3-methylxanthine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

16.8 g (0.7 mol) of sodium hydride were introduced in portions with stirring into a suspension of 99.6 g (0.6 mol) of 3-methylxanthine in 1.5 l of dimethylformamide. After evolution of hydrogen had ended, the mixture was heated to 100° C., treated dropwise with 76 g (0.6 mol) of benzyl chloride and heated at 120° C. for a further 6 hours. The reaction mixture was cooled and cautiously poured into 3 l of water. The solid was filtered off with suction and washed with water, the filter residue was taken up in ethanol and the solution was stirred at room temperature for one hour. The crystallizate was filtered, washed with ethanol and dried under reduced pressure.

後処理

  1. temperatureheated at 120° C. for a further 6 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationThe solid was filtered off with suction
  4. washwashed with water
  5. filtrationThe crystallizate was filtered
  6. washwashed with ethanol
  7. customdried under reduced pressure

出典と根拠

ORDレコード
ord-2b41b35df72e44c4adc18e6e041d2837
出典データセット
uspto-grants-1998_03
特許番号
US05728686

関連ノート

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