Methanol → AB-323/25048145

HRID 1467831ノート

反応式

HRID 1467831 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

HCID 816935AB-323/25048145収率 120.7%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c3672729829a4f6fb418ad75ae54003a
出典データセット
uspto-grants-2015_04
特許番号
US09000159B2

反応ノート

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