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

HRID 2258471노트

반응식

HRID 2258471 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-749580c4ed5446eba1aae9dfa34d8a4b
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05661153

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