氯化苄 → 7-苄基-3-甲基黄嘌呤

HRID 1995

反应方程式

HRID 1995 反应方程式
[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

参与物

7

反应物 4

HCID 7503氯化苄HCID 24758氢化钠HCID 706393-甲基黄嘌呤HCID 178418361HCID 178418361，化合物

产物 1

HCID 6856307-苄基-3-甲基黄嘌呤

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
100 °C

实验过程

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.

后处理

  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

来源与证据

ORD记录
ord-2b41b35df72e44c4adc18e6e041d2837
来源数据集
uspto-grants-1998_03
专利号
US05728686

关联笔记

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