Acetic Acid → 3-[4-Nitro-2-(trifluoromethyl)benzylidene]pentane-2,4-dione

HRID 1951387

반응식

HRID 1951387 반응식
[F:1][C:2]([F:15])([F:14])[C:3]1[CH:10]=[C:9]([N+:11]([O-:13])=[O:12])[CH:8]=[CH:7][C:4]=1[CH:5]=O.[CH3:16][C:17](=[O:22])[CH2:18][C:19](=[O:21])[CH3:20].C(O)(=O)C.N1CCCCC1>ClCCl>[N+:11]([C:9]1[CH:8]=[CH:7][C:4]([CH:5]=[C:18]([C:17](=[O:22])[CH3:16])[C:19](=[O:21])[CH3:20])=[C:3]([C:2]([F:15])([F:14])[F:1])[CH:10]=1)([O-:13])=[O:12]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 8082PiperidineHCID 31261AcetylacetoneHCID 123911054-Nitro-2-(trifluoromethyl)benzaldehyde

생성물 1

HCID 596030233-[4-Nitro-2-(trifluoromethyl)benzylidene]pentane-2,4-dione

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

1 g (4.56 mmol) of 2-trifluoromethyl-4-nitrobenzaldehyde, 0.51 ml (5.02 mmol) of 2,4-pentanedione, 0.4 ml (6.85 mmol) of acetic acid and 90 μl (0.91 mmol) of piperidine in 20 ml of anhydrous dichloromethane are stirred under reflux with a water trap for 24 h. After cooling, the reaction solution is washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution. The organic phase is dried over magnesium sulfate and concentrated. The residue (1.28 g) is reacted in the next stage without further purification.

후처리

  1. temperatureunder reflux with a water trap for 24 h
  2. temperatureAfter cooling
  3. washthe reaction solution is washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe residue (1.28 g) is reacted in the next stage without further purification

출처 및 근거

ORD 기록
ord-83ac0246cdb4453b984f57c40650b2e2
출처 데이터셋
uspto-grants-2013_03
특허 번호
US08404709B2

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