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Methanol → 2-([2-[(1-Methylethyl)oxy]ethyl}oxy)-8-(methoxy)-9-(tetrahydro-2H-Pyran-2-yl)-9H-purin-6-amine

HRID 1011048
ノート
印刷プレビュー

反応式

HRID 1011048 の反応式
[Na].Br[C:3]1[N:4]([CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21]2)[C:5]2[C:10]([N:11]=1)=[C:9]([NH2:12])[N:8]=[C:7]([O:13][CH2:14][CH2:15][O:16][CH:17]([CH3:19])[CH3:18])[N:6]=2.[CH3:26][OH:27]>>[CH3:18][CH:17]([O:16][CH2:15][CH2:14][O:13][C:7]1[N:6]=[C:5]2[C:10]([N:11]=[C:3]([O:27][CH3:26])[N:4]2[CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21]2)=[C:9]([NH2:12])[N:8]=1)[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 5360545SodiumHCID 576995988-bromo-2-({2-[(1-methylethyl)oxy]ethyl}oxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine

生成物 1

HCID 576996792-([2-[(1-Methylethyl)oxy]ethyl}oxy)-8-(methoxy)-9-(tetrahydro-2H-Pyran-2-yl)-9H-purin-6-amine

実験手順

To methanol (120 ml) was added sodium (0.966 g). When the metal was dissolved, 8-bromo-2-({2-[(1-methylethyl)oxy]ethyl}oxy)-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (5.69 g, 21.2 mmol) was added, heated to reflux and the solution stirred for 16 h, cooled to room temperature. The solvent was removed. Extracted with ethyl acetate after adding water, dried and concentrated to give the crude product which was purified through silica gel eluting with 2:1 ethyl acetate:petroleum ether to give the title compound (4.8 g).

後処理

  1. dissolutionWhen the metal was dissolved
  2. temperatureheated
  3. temperatureto reflux
  4. customThe solvent was removed
  5. extractionExtracted with ethyl acetate
  6. additionafter adding water
  7. customdried
  8. concentrationconcentrated
  9. customto give the crude product which
  10. customwas purified through silica gel eluting with 2:1 ethyl acetate

出典と根拠

ORDレコード
ord-9a8e7c41a71e4a0b95d25833b43c1cb7
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07977344B2

反応ノート

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