HCID 10584109、化合物 → HCID 10584991、化合物

HRID 1744765

反応式

HRID 1744765 の反応式
[NH2:1][C:2]1[C:3](=[O:14])[NH:4][C:5](=[O:13])[N:6]([CH2:9][CH:10]([CH3:12])[CH3:11])[C:7]=1[NH2:8].[CH:15](S([O-])(=O)=O)(O)[CH:16](S([O-])(=O)=O)O.O.[Na+].[Na+]>Cl>[CH2:9]([N:6]1[C:7]2[C:2](=[N:1][CH:15]=[CH:16][N:8]=2)[C:3](=[O:14])[NH:4][C:5]1=[O:13])[CH:10]([CH3:11])[CH3:12]

参加物

4

反応物 2

HCID 10584109HCID 10584109、化合物HCID 16211366Disodium 1,2-dihydroxy-1,2-ethanedisulfonate monohydrate

生成物 1

HCID 10584991HCID 10584991、化合物収率 19.3%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

After dissolving 19.8 g (100 mmol) 5,6-diamino-1-isobutyluracil in 1 liter of 1N HCl at 70° C., 186.3 g of glyoxal sodium bisulfite addition compound hydrate was added and the mixture refluxed for 1 hour. After extracting the mixture several times with ethyl acetate, the collected ethyl acetate fractions were washed with water, dried over MgSO4 and evaporated. The crude product was purified by preparative column chromatography using chloroform/methanol 9:1 as eluant yielding 4.25 g (18%) of 1-isobutyl-1H-pteridine-2,4-dione (m.p. 200–201° C., Lit. 195–197° C.).

後処理

  1. temperaturethe mixture refluxed for 1 hour
  2. extractionAfter extracting the mixture several times with ethyl acetate
  3. washthe collected ethyl acetate fractions were washed with water
  4. dry with materialdried over MgSO4
  5. customevaporated
  6. customThe crude product was purified by preparative column chromatography

出典と根拠

ORDレコード
ord-64f1a6ecd221468b9d26aa84a2812744
出典データセット
uspto-grants-2006_03
特許番号
US07018786B2

関連ノート

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