Hydrochloric Acid → 6-Amino-2-{[(1S)-1-methylbutyl]oxy}-9-[4-(tetrahydro-2H-pyran-4-ylamino)butyl]-7,9-dihydro-8H-purin-8-one

HRID 2036367ノート

反応式

HRID 2036367 の反応式
[CH3:1][C@H:2]([O:6][C:7]1[N:15]=[C:14]2[C:10]([N:11]=[C:12]([O:27]C)[N:13]2[CH2:16][CH2:17][CH2:18][CH2:19][NH:20][CH:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)=[C:9]([NH2:29])[N:8]=1)[CH2:3][CH2:4][CH3:5].Cl.O1CCOCC1>CO>[NH2:29][C:9]1[N:8]=[C:7]([O:6][C@@H:2]([CH3:1])[CH2:3][CH2:4][CH3:5])[N:15]=[C:14]2[C:10]=1[NH:11][C:12](=[O:27])[N:13]2[CH2:16][CH2:17][CH2:18][CH2:19][NH:20][CH:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 582909342-{[(1S)-1-Methylbutyl]oxy}-8-(methyloxy)-9-[4-(tetrahydro-2H-pyran-4-ylamino)butyl]-9H-purin-6-amine

生成物 1

HCID 672251926-Amino-2-{[(1S)-1-methylbutyl]oxy}-9-[4-(tetrahydro-2H-pyran-4-ylamino)butyl]-7,9-dihydro-8H-purin-8-one収率 96.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

2-{[(1S)-1-Methylbutyl]oxy}-8-(methyloxy)-9-[4-(tetrahydro-2H-pyran-4-ylamino)butyl]-9H-purin-6-amine (30.35 mg, 0.075 mmol) was dissolved in methanol (2.0 ml) and treated with 4M HCl in 1,4 dioxane (0.467 ml, 1.866 mmol) and stirred in a capped vial over the weekend. The solvent was evaporated under nitrogen and the residue was dissolved in methanol and passed down an aminopropyl SPE cartridge (2 g, pre-conditioned with 2 column volumes of methanol) and washed through with 1 column volume of methanol. The eluant was evaporated under nitrogen in a blowdown unit to give the title compound as an off-white solid (28.34 mg).

後処理

  1. customThe solvent was evaporated under nitrogen
  2. dissolutionthe residue was dissolved in methanol
  3. washwashed through with 1 column volume of methanol
  4. customThe eluant was evaporated under nitrogen in a blowdown unit

出典と根拠

ORDレコード
ord-edd61e910a19472580e59bd8337e67b7
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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