4-Hydroxybenzaldehyde → HCID 17859705, 화합물

HRID 347675노트

반응식

HRID 347675 반응식
[Cl:1][C:2]1[N:3]=[N:4][C:5](Cl)=[CH:6][CH:7]=1.[OH:9][C:10]1[CH:17]=[CH:16][C:13]([CH:14]=[O:15])=[CH:12][CH:11]=1.C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[Cl:1][C:2]1[N:3]=[N:4][C:5]([O:9][C:10]2[CH:17]=[CH:16][C:13]([CH:14]=[O:15])=[CH:12][CH:11]=2)=[CH:6][CH:7]=1

참가 물질

6

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 6228DimethylformamideHCID 11430Potassium CarbonateHCID 673313,6-Dichloropyridazine

생성물 1

HCID 17859705HCID 17859705, 화합물수율 86.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

3,6-Dichloropyridazine (3.00 g, 20.1 mmol), 4-hydroxybenzaldehyde (2.46 g, 20.1 mmol), potassium carbonate (2.78 g, 20.1 mmol) and 60 mL of N,N-dimethylformamide were mixed and the mixture was refluxed for 1 hour. The reaction mixture was poured into water, which was extracted with ethyl acetate. The extracted solution was washed with brine, then dried over anhydrous magnesium sulfate and concentrated. The residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=1:1 v/v) to obtain 4.06 g (86%) of the title compound as colorless crystalline powder.

후처리

  1. temperaturethe mixture was refluxed for 1 hour
  2. extractionwas extracted with ethyl acetate
  3. washThe extracted solution was washed with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel chromatography (eluate n-hexane:ethyl acetate=1:1 v/v)

출처 및 근거

ORD 기록
ord-3b8cfaeaaf8c4c44af8c190641179feb
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07176204B2

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