Acetic Acid → 6-Amino-3-methyl-5-nitroso-1-phenylpyrimidine-2,4(1H,3H)-dione

HRID 2258471ノート

反応式

HRID 2258471 の反応式
[NH2:1][C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[CH:3]=1.[OH-].[Na+].[N:19]([O-])=[O:20].[Na+].C(O)(=O)C>O>[NH2:1][C:2]1[N:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[C:6](=[O:14])[N:5]([CH3:15])[C:4](=[O:16])[C:3]=1[N:19]=[O:20]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 14798Sodium HydroxideHCID 16492566-Amino-3-methyl-1-phenylpyrimidine-2,4(1H,3H)-dioneHCID 23668193Sodium Nitrite

生成物 1

HCID 127062666-Amino-3-methyl-5-nitroso-1-phenylpyrimidine-2,4(1H,3H)-dione収率 99.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

The obtained 6-amino-3-methyl-1-phenyluracil (24 g, 0.11M) and NaOH (2.8 g, 70 mM) were dissolved in 110 ml of water. To the resulting solution was added dropwise an aqueous solution of sodium nitrite (9.5 g/80 ml). Acetic acid (13 ml) was then added dropwise at 0° C. and the mixture was brought to room temperature, followed by stirring for 2 hours. A precipitated solid product was obtained by filtration. The solid product was washed successively with water and methanol and dried to yield 6-amino-3-methyl-5-nitroso-1-phenyluracil (yield: 27 g, or 99% based on 6-amino-3-methyl-1-phenyluracil).

後処理

  1. customwas brought to room temperature
  2. customA precipitated solid product was obtained by filtration
  3. washThe solid product was washed successively with water and methanol
  4. customdried

出典と根拠

ORDレコード
ord-749580c4ed5446eba1aae9dfa34d8a4b
出典データセット
uspto-grants-1997_08
特許番号
US05661153

反応ノート

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