Hydrochloric Acid → 6-Amino-2-butylamino-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011154ノート

反応式

HRID 1011154 の反応式
[CH2:1]([NH:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:22]C)[N:12]2[CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][O:18][CH2:17]2)=[C:8]([NH2:24])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.[OH-].[Na+]>CO.O1CCOCC1>[NH2:24][C:8]1[N:7]=[C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:22])[N:12]2[CH2:15][CH:16]1[CH2:21][CH2:20][CH2:19][O:18][CH2:17]1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57699736N2-Butyl-8-methoxy-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purine-2,6-diamine

生成物 1

HCID 250251666-Amino-2-butylamino-9-(tetrahydro-2H-pyran-3-ylmethyl)-7,9-dihydro-8H-Purin-8-one収率 58%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of N2-butyl-8-methoxy-9-(tetrahydro-2H-pyran-3-ylmethyl)-9H-purine-2,6-diamine (45 mg) in dry methanol (3 ml) at room temperature and under nitrogen was added 4.0M hydrogen chloride in 1,4-dioxane (0.7 ml) in one go. The reaction was left to stir at room temperature for 3 hours. The reaction was neutralised by the addition of 2.0M sodium hydroxide solution and concentrated in vacuo. The residue was taken up in water (5 ml) and the solid filtered and dried in vacuo (60° C.) for 30 minutes. This afforded the title compound as a solid (25 mg).

後処理

  1. waitThe reaction was left
  2. concentrationconcentrated in vacuo
  3. filtrationthe solid filtered
  4. customdried in vacuo (60° C.) for 30 minutes

出典と根拠

ORDレコード
ord-31cba9359a184899b047064ebac93e32
出典データセット
uspto-grants-2011_07
特許番号
US07977344B2

反応ノート

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