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

HRID 421306ノート

反応式

HRID 421306 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-15f28acd93234464a79583052c66f7fb
出典データセット
uspto-grants-2012_01
特許番号
US08097622B2

反応ノート

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