Methanol → AB-323/25048145

HRID 467861노트

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HRID 467861 반응식
[N+:1]([C:4]1[C:5](=[O:14])[N:6]([CH3:13])[C:7](=[O:12])[N:8]([CH3:11])[C:9]=1[CH3:10])([O-])=O.CO>[Pd].C1(C)C=CC=CC=1>[NH2:1][C:4]1[C:5](=[O:14])[N:6]([CH3:13])[C:7](=[O:12])[N:8]([CH3:11])[C:9]=1[CH3:10]

참가 물질

5

반응물 2

HCID 887MethanolHCID 7503695-Nitro-1,3,6-trimethyluracil

생성물 1

HCID 816935AB-323/25048145수율 120.7%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 1140Toluene용매

실험 절차

To a stirred suspension of 5-nitro-1,3,6-trimethylpyrimidine-2,4(1H,3H)-dione (4.2 g, 20.084 mmol) in 1:1 mixture of methanol and toluene (200 ml) was added 10% Pd—C (1.2 g). The reaction mixture was stirred under hydrogen atmosphere at room temperature overnight. The mixture was then filtered over a celite bed and was thoroughly washed with methanol (200 ml). The filtrate was collected and evaporated to give viscous residue which was then purified by column chromatography to afford 4.1 g of the product as an off-white solid.

후처리

  1. filtrationThe mixture was then filtered over a celite bed
  2. washwas thoroughly washed with methanol (200 ml)
  3. customThe filtrate was collected
  4. customevaporated
  5. customto give viscous residue which
  6. customwas then purified by column chromatography

출처 및 근거

ORD 기록
ord-48db6a730ee441a18f60baaf858d0332
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08623880B2

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