Water → Aditeren

HRID 462526

反応式

HRID 462526 の反応式
O.[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([CH2:10][C:11]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([NH2:19])=[C:13]([O:20][CH3:21])[CH:12]=2)=[C:5](Cl)[N:4]=1>[Hg](Cl)Cl.[Zn].C(O)(=O)C>[NH2:2][C:3]1[N:8]=[C:7]([NH2:9])[C:6]([CH2:10][C:11]2[CH:12]=[C:13]([O:20][CH3:21])[C:14]([NH2:19])=[C:15]([O:17][CH3:18])[CH:16]=2)=[CH:5][N:4]=1

参加物

6

反応物 2

HCID 962WaterHCID 21280993HCID 21280993、化合物

生成物 1

HCID 176875Aditeren

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 24085Mercuric Chloride触媒HCID 176Acetic Acid溶媒

実験手順

A solution of 0.1 g. of mercury (II) chloride in 2 ml. of water and 1.5 g. of zinc powder was added to a solution of 1.5 g. of 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-6-chloropyrimidine in 15.5 ml. of glacial acetic acid and the mixture was boiled under reflux with stirring overnight. Then, the mixture was filtered while hot and the zinc powder washed with 5 ml. of acetic acid. The combined filtrates were added dropwise with stirring at a temperature below 20° C. to 40 ml. of concentrated ammonia. Then, the mixture was stirred at 20° C. for an additional hour and the solid material was removed by filtration under vacuum, washed with water, dried, recrystallized from methanol and there was obtained 2,4-diamino-5-(4-amino-3,5-dimethoxy-benzyl)-pyrimidine having a melting point of 214° C.

後処理

  1. temperatureunder reflux
  2. filtrationThen, the mixture was filtered while hot and the zinc powder
  3. washwashed with 5 ml
  4. additionThe combined filtrates were added dropwise
  5. stirringwith stirring at a temperature below 20° C. to 40 ml
  6. stirringThen, the mixture was stirred at 20° C. for an additional hour
  7. customthe solid material was removed by filtration under vacuum
  8. washwashed with water
  9. customdried
  10. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-299ac4868f0c4bd7a5ae90f14d411515
出典データセット
uspto-grants-1985_05
特許番号
US04515948

関連ノート

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