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

HRID 1739424노트

반응식

HRID 1739424 반응식
[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]

참가 물질

8

반응물 4

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

생성물 1

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

시약·촉매·용매 3

HCID 175Acetate용매HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-522548265d3c443e84545689190ffc0b
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05965730

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