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Hydrochloric Acid → 6-amino-1-benzyl-5-nitrosopyrimidine-2,4(1H,3H)-dione

HRID 489472
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HRID 489472 반응식
[NH2:1][C:2]1[N:7]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:6](=[O:15])[NH:5][C:4](=[O:16])[CH:3]=1.[N:17]([O-])=[O:18].[Na+].Cl>CN(C)C=O.O>[NH2:1][C:2]1[N:7]([CH2:8][C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[C:6](=[O:15])[NH:5][C:4](=[O:16])[C:3]=1[N:17]=[O:18]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 2507466-Amino-1-benzyluracilHCID 23668193Sodium Nitrite

생성물 1

HCID 33071146-amino-1-benzyl-5-nitrosopyrimidine-2,4(1H,3H)-dione

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

To a solution of 6-amino-1-benzyl-1,3-dihydropyrimidine-2,4-dione (2.0 g, 9.2 mmol) in a mixture of 15 ml of N,N-dimethylformamide and 5 ml of water at 90° C. was added sodium nitrite (1.27 g, 69 mmol). To this reaction mixture was added concentrated hydrochloric acid until there was no deepening of color, and the mixture was heated at 70° C. for 1 hour. The solvent was removed under reduced pressure, the residue dissolved in water, and concentrated hydrochloric acid added to produce a pH of 4.0. The precipitate was filtered off, washed with water, and dried under reduced pressure, to provide 6-amino-5-nitroso-1-benzyl-1,3-dihydropyrimidine-2,4-dione, a compound of formula (24).

후처리

  1. customThe solvent was removed under reduced pressure
  2. dissolutionthe residue dissolved in water
  3. additionconcentrated hydrochloric acid added
  4. customto produce a pH of 4.0
  5. filtrationThe precipitate was filtered off
  6. washwashed with water
  7. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-de0ba5501863471eaafda2a660bcd22d
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06977300B2

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