Benzyl Chloride → 7-Benzyl-3-methylxanthine

HRID 1995

반응식

HRID 1995 반응식
[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

참가 물질

7

반응물 4

HCID 7503Benzyl ChlorideHCID 24758Sodium hydrideHCID 706393-MethylxanthineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 6856307-Benzyl-3-methylxanthine

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2b41b35df72e44c4adc18e6e041d2837
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05728686

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