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Methyl iodide → 8-Bromo-3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione

HRID 1754585
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HRID 1754585 반응식
[Br:1][C:2]1[NH:10][C:9]2[C:8](=[O:11])[NH:7][C:6](=O)[N:5]([CH3:13])[C:4]=2[N:3]=1.[CH3:14]I.[C:16](=[O:19])([O-])[O-].[K+].[K+]>CN(C)C=O.O>[Br:1][C:2]1[N:10]([CH3:14])[C:9]2[C:8](=[O:11])[N:7]([CH3:6])[C:16](=[O:19])[N:5]([CH3:13])[C:4]=2[N:3]=1
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참가 물질

6

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 15487978-bromo-3-methyl-3,7-dihydro-1H-purine-2,6-dione

생성물 1

HCID 641278-Bromo-3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
60 °C

실험 절차

A solution of 8-bromo-3-methyl xanthine (300 mg; 1.2 mmol) and methyl iodide (1.42 g; 10.0 mmol) in N,N-dimethylformamide (5 ml) was added to potassium carbonate (662 mg; 4.8 mmol) and was heated to 60° C. for 6 hrs. The reaction mixture was poured in water (25 ml) and extracted with ethyl acetate (3×25 ml). The combined extract was dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The product was purified by flash chromatography over silica gel eluting with ethyl acetate to yield the desired product. 315 mg; 92% PRO-04-45

후처리

  1. extractionextracted with ethyl acetate (3×25 ml)
  2. extractionThe combined extract
  3. dry with materialwas dried over anhydrous magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe product was purified by flash chromatography over silica gel eluting with ethyl acetate

출처 및 근거

ORD 기록
ord-c261131c51f64b10a72372ceb4d21ba8
출처 데이터셋
uspto-grants-2015_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09169255B2

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