Hydrogen Peroxide → HCID 53681338、化合物

HRID 481308

反応式

HRID 481308 の反応式
[Cl:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=[O:9])[CH:5]=[CH:4][CH:3]=1.[OH:11]O>FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:3]=[CH:4][CH:5]=[C:6]([C:8]([OH:10])=[O:9])[N+:7]=1[O-:11]

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 208126-Chloropicolinic acid

生成物 1

HCID 53681338HCID 53681338、化合物収率 67%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To a solution of 6-chloro-2-pyridinecarboxylic acid (14.8 g, 0.093 mol, for preparation, see Delarge, II. Farmaco-Ed.Sc., 1967, 22, 1069) in trifluoroacetic acid (110 ml) was added 75 ml of 30% aqueous hydrogen peroxide solution. The mixture was heated to 60° for 2 hours, cooled to room temperature and poured onto ice water. The white precipitate was filtered and was washed well with water to yield 10.8 g (67%) of the title compound of this preparation. mp 168°-170° C. 1H NMR (CDCl3): δ 7.46 (1H, d, J=8), 7.77 (1H, dd, J=8, 8), 8.01 (1H, d, J=8).

後処理

  1. temperatureThe mixture was heated to 60° for 2 hours
  2. additionpoured onto ice water
  3. filtrationThe white precipitate was filtered
  4. washwas washed well with water
  5. customto yield

出典と根拠

ORDレコード
ord-19fb74ca5ccc480c85a1d82d3c14c559
出典データセット
uspto-grants-1998_08
特許番号
US05789408

関連ノート

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