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1-Butanol → 6-Amino-2-[(cyclohexylmethyl)amino]-9-(tetrahydro-2H-Pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011184
ノート
印刷プレビュー

反応式

HRID 1011184 の反応式
Br[C:2]1[N:3]([CH2:20][CH:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[C:4]2[C:9]([N:10]=1)=[C:8]([NH2:11])[N:7]=[C:6]([NH:12][CH2:13][CH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1)[N:5]=2.Cl.C([OH:32])CCC>>[NH2:11][C:8]1[N:7]=[C:6]([NH:12][CH2:13][CH:14]2[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]2)[N:5]=[C:4]2[C:9]=1[NH:10][C:2](=[O:32])[N:3]2[CH2:20][CH:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1
参加物反応条件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 2631-ButanolHCID 313Hydrochloric AcidHCID 576996278-Bromo-N2-(cyclohexylmethyl)-9-(tetrahydro-2H-Pyran-4-ylmethyl)-9H-Purine-2,6-diamine

生成物 1

HCID 576997146-Amino-2-[(cyclohexylmethyl)amino]-9-(tetrahydro-2H-Pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one

反応条件

温度
100 °C

実験手順

To a solution of 8-bromo-N2-(cyclohexylmethyl)-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine-2,6-diamine (110 mg) in dry n-butanol (1.5 ml) was added 37% grade hydrochloric acid (1.5 ml) at RT. The reaction was heated to 100° C. for six hours. The reaction was concentrated in vacuo, taken up in water (5 ml) and neutralised by the addition of 2.0M sodium hydroxide solution. The resulting white precipitate was filtered. This was purified by C18 reverse phase chromatography using water (containing 0.1% formic acid)-acetonitrile (containing 0.05% formic acid) as eluant (20-60%) to afford a white solid (20 mg).

後処理

  1. concentrationThe reaction was concentrated in vacuo
  2. additionneutralised by the addition of 2.0M sodium hydroxide solution
  3. filtrationThe resulting white precipitate was filtered
  4. customThis was purified by C18 reverse phase chromatography

出典と根拠

ORDレコード
ord-ff3e7eb1553b4c76a40b7d999a2a8d6a
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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