Hydrochloric Acid → 6-Amino-2-(butyloxy)-9-{3-[(tetrahydro-3-furanylmethyl)amino]propyl}-7,9-dihydro-8H-purin-8-one

HRID 2036366ノート

反応式

HRID 2036366 の反応式
[CH2:1]([O:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:25]C)[N:12]2[CH2:15][CH2:16][CH2:17][NH:18][CH2:19][CH:20]2[CH2:24][CH2:23][O:22][CH2:21]2)=[C:8]([NH2:27])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.O1CCOCC1>CO>[NH2:27][C:8]1[N:7]=[C:6]([O:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:25])[N:12]2[CH2:15][CH2:16][CH2:17][NH:18][CH2:19][CH:20]1[CH2:24][CH2:23][O:22][CH2:21]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 67224141HCID 67224141、化合物

生成物 1

HCID 672115066-Amino-2-(butyloxy)-9-{3-[(tetrahydro-3-furanylmethyl)amino]propyl}-7,9-dihydro-8H-purin-8-one収率 53%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

2-(Butyloxy)-8-(methyloxy)-9-{3-[(tetrahydro-3-furanylmethyl)amino]propyl}-9H-purin-6-amine (11 mg, 0.029 mmol) and 4M HCl in 1,4 dioxane (0.160 ml, 0.639 mmol) were stirred at 20° C. for 16 hours in methanol (1 ml). The solvent was removed by N2 blowdown. The sample was loaded in methanol and purified by SPE on an aminopropyl (NH2) cartridge (2 g) using methanol. The appropriate fractions were combined and dried under a stream of nitrogen to give the crude product as a white solid. The sample were dissolved in 1:1 MeOH:DMSO (1 ml) and purified by Mass Directed AutoPrep (Method A). The solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus to give the title compound as a white solid (5.6 mg).

後処理

  1. customThe solvent was removed by N2
  2. custompurified by SPE on an aminopropyl (NH2) cartridge (2 g)
  3. customdried under a stream of nitrogen
  4. customto give the crude product as a white solid
  5. customDMSO (1 ml) and purified by Mass Directed AutoPrep (Method A)
  6. customThe solvent was dried under a stream of nitrogen in the Radleys blowdown apparatus

出典と根拠

ORDレコード
ord-245b607e6d2247e9803acedea409e7aa
出典データセット
uspto-grants-2013_11
特許番号
US08575181B2

反応ノート

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