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Hydrochloric Acid → 6-Amino-2-({2-[(1-methylethyl)oxy]ethyl}oxy)-9-(tetrahydro-2H-pyran-4-ylmethyl)-7,9-dihydro-8H-purin-8-one

HRID 1011193
ノート
印刷プレビュー

反応式

HRID 1011193 の反応式
[CH3:1][CH:2]([O:4][CH2:5][CH2:6][O:7][C:8]1[N:16]=[C:15]2[C:11]([N:12]=[C:13]([O:24]C)[N:14]2[CH2:17][CH:18]2[CH2:23][CH2:22][O:21][CH2:20][CH2:19]2)=[C:10]([NH2:26])[N:9]=1)[CH3:3].Cl.[OH-].[Na+]>CO.O1CCOCC1>[NH2:26][C:10]1[N:9]=[C:8]([O:7][CH2:6][CH2:5][O:4][CH:2]([CH3:3])[CH3:1])[N:16]=[C:15]2[C:11]=1[NH:12][C:13](=[O:24])[N:14]2[CH2:17][CH:18]1[CH2:23][CH2:22][O:21][CH2:20][CH2:19]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57699826HCID 57699826、化合物

生成物 1

HCID 576996306-Amino-2-({2-[(1-methylethyl)oxy]ethyl}oxy)-9-(tetrahydro-2H-pyran-4-ylmethyl)-7,9-dihydro-8H-purin-8-one収率 75.6%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

To a solution of 2-({2-[(1-methylethyl)oxy]ethyl}oxy)-8-(methoxy)-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purin-6-amine (165 mg) in dry methanol (17 ml) was added 4.0M hydrogen chloride in 1,4-dioxane (2.95 ml) in one go. The reaction was left to stir at room temperature for 5 hours. The reaction was neutralised by the addition of 2.0M sodium hydroxide solution and concentrated in vacuo to give an off-white solid. The solid was triturated in water, and filtered under vacuum, washing with more water, to give an off-white solid (120 mg).

後処理

  1. waitThe reaction was left
  2. concentrationconcentrated in vacuo
  3. customto give an off-white solid
  4. customThe solid was triturated in water
  5. filtrationfiltered under vacuum
  6. washwashing with more water

出典と根拠

ORDレコード
ord-0ed9fc2681fa470e9b07396cb2458a41
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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