Hydrochloric Acid → 3,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzoic acid

HRID 1739424ノート

反応式

HRID 1739424 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:8]([C:13](=[O:21])[C:14]2[CH:19]=[CH:18][N:17]=[C:16]([Br:20])[CH:15]=2)=[CH:9][C:10]=1[O:11][CH3:12])[CH:6]=[O:7].C1(C=CC=C(O)C=1)[OH:23].Cl[O-].[Na+].Cl>O1CCOCC1.C([O-])(=O)C.O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:8]([C:13](=[O:21])[C:14]2[CH:19]=[CH:18][N:17]=[C:16]([Br:20])[CH:15]=2)=[CH:9][C:10]=1[O:11][CH3:12])[C:6]([OH:23])=[O:7]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 5054ResorcinolHCID 218408403,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzaldehydeHCID 23665760Sodium Hypochlorite

生成物 1

HCID 218408063,4-Dimethoxy-6-(2-bromoisonicotinoyl)benzoic acid収率 89.6%

試薬・触媒・溶媒 3

HCID 175Acetate溶媒HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 3,4-dimethoxy-6-(2-bromoisonicotinoyl)benzaldehyde (8.61 g) in dioxane (120 ml) is added dropwise a solution of resorcinol (3.25 g) in acetate buffer (pH 3.8, 60 ml) at room temperature. To the mixture is Gradually added dropwise an aqueous solution of sodium hypochlorite (3.1 g) in water (30 ml), and the mixture is stirred at room temperature for two hours. The pH value of the reaction mixture is adjusted to about pH 1 with conc. hydrochloric acid, and then extracted with chloroform. The extract is washed, dried, and concentrated to give 3,4-dimethoxy-6-(2-bromoisonicotinoyl)benzoic acid (8.07 g).

後処理

  1. extractionextracted with chloroform
  2. washThe extract is washed
  3. customdried
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-522548265d3c443e84545689190ffc0b
出典データセット
uspto-grants-1999_10
特許番号
US05965730

反応ノート

読み込み中…