Water → Aditeren

HRID 462526

반응식

HRID 462526 반응식
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

참가 물질

6

반응물 2

HCID 962WaterHCID 21280993HCID 21280993, 화합물

생성물 1

HCID 176875Aditeren

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 24085Mercuric Chloride촉매HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-299ac4868f0c4bd7a5ae90f14d411515
출처 데이터셋
uspto-grants-1985_05
특허 번호
US04515948

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