Nitric Acid → HCID 12130786、化合物

HRID 581917ノート

反応式

HRID 581917 の反応式
[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]

参加物

4

反応物 3

HCID 944Nitric AcidHCID 1118Sulfuric Acid2 回HCID 189234-Phenylpyrimidine

生成物 1

HCID 12130786HCID 12130786、化合物収率 50%

反応条件

温度
0 °C

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-b8b721cdadab41be81c95df26252b943
出典データセット
uspto-grants-1999_07
特許番号
US05922725

反応ノート

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