HCID 10584109, 화합물 → HCID 10584991, 화합물

HRID 1744765

반응식

HRID 1744765 반응식
[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]

참가 물질

4

반응물 2

HCID 10584109HCID 10584109, 화합물HCID 16211366Disodium 1,2-dihydroxy-1,2-ethanedisulfonate monohydrate

생성물 1

HCID 10584991HCID 10584991, 화합물수율 19.3%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-64f1a6ecd221468b9d26aa84a2812744
출처 데이터셋
uspto-grants-2006_03
특허 번호
US07018786B2

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