Acetylacetone → HCID 178468324, 화합물

HRID 1407067

반응식

HRID 1407067 반응식
[F:1][CH:2]([F:11])[O:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH2:6].[N:12]([O-])=O.[Na+].C([O-])(=O)C.[Na+].[C:21]([CH2:24][C:25](=[O:27])[CH3:26])(=[O:23])[CH3:22]>C(O)(=O)C.Cl.O.C(O)C>[F:1][CH:2]([F:11])[O:3][C:4]1[CH:10]=[CH:9][CH:8]=[CH:7][C:5]=1[NH:6][N:12]=[C:24]([C:25](=[O:27])[CH3:26])[C:21](=[O:23])[CH3:22]

참가 물질

9

반응물 4

HCID 31261AcetylacetoneHCID 517045Sodium AcetateHCID 9346202-(Difluoromethoxy)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 178468324HCID 178468324, 화합물수율 94.1%

시약·촉매·용매 4

HCID 176Acetic Acid용매HCID 313Hydrochloric Acid용매HCID 702Ethanol용매HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

To a solution of 2-(difluoromethoxy)aniline (1000 mg, 6.25 mmol) in 15 mL of acetic acid and 2.5 mL of concentrated hydrochloride solution, sodium nitrite (518 mg, 7.50 mmol) in 4 mL of water was added dropwise at 0° C., and the mixture was stirred at 0° C. for 1 h. Then to the reaction mixture was added dropwise a solution of sodium acetate (1538 mg, 18.75 mmol) and acetylacetone (812 mg, 8.12 mmol) in 10 mL of ethanol and 6 mL of water. The mixture was stirred at room temperature overnight, filtered, washed with water, EtOH/H2O (1:1) and hexane, and dried to give 3-{[2-(difluoromethoxy)phenyl]hydrazono}pentane-2,4-dione (1590 mg, 94%).

후처리

  1. stirringThe mixture was stirred at room temperature overnight
  2. filtrationfiltered
  3. washwashed with water, EtOH/H2O (1:1) and hexane
  4. customdried

출처 및 근거

ORD 기록
ord-1a5b23f14fbf4e4ba58f8efaaffeee67
출처 데이터셋
uspto-grants-2014_12
특허 번호
US08916566B2

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