Morpholine → 2-Chloro-6-morpholin-4-yl-9-(tetrahydrofuran-3-ylmethyl)-9H-purine

HRID 1876496노트

반응식

HRID 1876496 반응식
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH:12]2[CH2:16][CH2:15][O:14][CH2:13]2)=[C:4](Cl)[N:3]=1.[NH:18]1[CH2:23][CH2:22][O:21][CH2:20][CH2:19]1>C(O)C>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[CH2:11][CH:12]2[CH2:16][CH2:15][O:14][CH2:13]2)=[C:4]([N:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)[N:3]=1

참가 물질

4

반응물 2

HCID 8083MorpholineHCID 593335962,6-Dichloro-9-(tetrahydrofuran-3-ylmethyl)-9H-purine

생성물 1

HCID 593335062-Chloro-6-morpholin-4-yl-9-(tetrahydrofuran-3-ylmethyl)-9H-purine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2,6-Dichloro-9-(tetrahydrofuran-3-ylmethyl)-9H-purine (41 g) was dissolved in ethanol (200 ml) followed by the addition of morpholine (20 ml) and the resulting mixture was heated to reflux for 2 hours. The solvent was evaporated under reduced pressure, the residue was partitioned with ethyl acetate and saturated aqueous sodium bicarbonate solution, and the organic layer was washed with water and dried over magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (hexane:ethyl acetate, 5:5 to 2:8 to 0:10) to give the title compound (41 g) as a white solid.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux for 2 hours
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was partitioned with ethyl acetate and saturated aqueous sodium bicarbonate solution
  5. washthe organic layer was washed with water
  6. dry with materialdried over magnesium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customthe residue was purified by silica gel chromatography (hexane:ethyl acetate, 5:5 to 2:8 to 0:10)

출처 및 근거

ORD 기록
ord-44617dc926b840e5966c680401a377ce
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08309546B2

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