N6-Methyladenine → N6-methyl-9-[3-(4-phenyl-piperazino)-propyl]-adenine

HRID 1973236노트

반응식

HRID 1973236 반응식
[Na].[CH3:2][NH:3][C:4]1[N:12]=[CH:11][N:10]=[C:9]2[C:5]=1[NH:6][CH:7]=[N:8]2.[C:13]1([N:19]2[CH2:24][CH2:23][N:22]([CH2:25][CH2:26][CH2:27]Cl)[CH2:21][CH2:20]2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>C(O)(C)C>[CH3:2][NH:3][C:4]1[N:12]=[CH:11][N:10]=[C:9]2[C:5]=1[N:6]=[CH:7][N:8]2[CH2:27][CH2:26][CH2:25][N:22]1[CH2:23][CH2:24][N:19]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH2:20][CH2:21]1

참가 물질

5

반응물 3

HCID 67955N6-MethyladenineHCID 139197Piperazine, 1-(3-chloropropyl)-4-phenyl-HCID 5360545Sodium

생성물 1

HCID 86734243N6-methyl-9-[3-(4-phenyl-piperazino)-propyl]-adenine수율 45.1%

시약·촉매·용매 1

HCID 3776Isopropanol용매2회

실험 절차

1.38 g (0.06 mole) of sodium are dissolved in 120 ml of isopropanol. 8.9 g (0.06 mole) of N6 -methyl-adenine are added to this solution, which is then heated under reflux for 10 minutes, cooled and 15.8 g (0.066 mole) of 3-(4-phenyl-piperazino)-propyl chloride in 30 ml of isopropanol are added thereto. This reaction mixture is heated under reflux for 6 hours. Thereafter, it is cooled, suction filtered and sodium chloride washed out from the residue with water. After washing with water and drying, the product is recrystallized from isopropanol. There are obtained 9.5 g (45% of theory) of N6 -methyl-9-[3-(4-phenyl-piperazino)-propyl]-adenine, which has a melting point of 162°-163° C.

후처리

  1. temperatureis then heated
  2. temperatureunder reflux for 10 minutes
  3. temperaturecooled
  4. temperatureThis reaction mixture is heated
  5. temperatureunder reflux for 6 hours
  6. temperatureThereafter, it is cooled
  7. filtrationsuction filtered
  8. washsodium chloride washed out from the residue with water
  9. washAfter washing with water
  10. customdrying
  11. customthe product is recrystallized from isopropanol

출처 및 근거

ORD 기록
ord-0bc1cf3c13ec47ff995bf95cc035ab77
출처 데이터셋
uspto-grants-1976_12
특허 번호
US03996361

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