Nitric Acid → HCID 12130786, 화합물

HRID 581917노트

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HRID 581917 반응식
[C:1]1([C:7]2[CH:12]=[CH:11][N:10]=[CH:9][N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.OS(O)(=O)=O.[N+:18]([O-])([OH:20])=[O:19]>>[N+:18]([C:5]1[CH:6]=[C:1]([C:7]2[CH:12]=[CH:11][N:10]=[CH:9][N:8]=2)[CH:2]=[CH:3][CH:4]=1)([O-:20])=[O:19]

참가 물질

4

반응물 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2회HCID 189234-Phenylpyrimidine

생성물 1

HCID 12130786HCID 12130786, 화합물수율 50%

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온도
0 °C

실험 절차

A mixture of 4-phenylpyrimidine (10 g, 64 mmol) and conc. H2SO4 (33 ml) was added to a mixture of conc. H2SO4 (22 ml) and conc. HNO3 (16 ml) at 0° C. The resulting mixture was stirred at 0° C. for 2 hr, poured onto crushed ice, and extracted with CH2Cl2. The extract was washed with a 5% aqueous NaHCO3 solution, dried over MgSO4 and concentrated under reduced pressure. The residue was triturated with isopropanol and the precipitate was filtered off and dried under reduced pressure to give (57) (6.4 g, 50%).

후처리

  1. additionpoured
  2. customonto crushed ice
  3. extractionextracted with CH2Cl2
  4. washThe extract was washed with a 5% aqueous NaHCO3 solution
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was triturated with isopropanol
  8. filtrationthe precipitate was filtered off
  9. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-b8b721cdadab41be81c95df26252b943
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922725

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