Piperidine → HCID 76211114, 화합물

HRID 38301

반응식

HRID 38301 반응식
[C:1]([C:4]1[C:5](=[O:15])[O:6][C:7]2[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=2[C:9]=1[OH:10])(=[O:3])[CH3:2].[Cl:16][C:17]1[CH:18]=[C:19]([CH:22]=[CH:23][C:24]=1[O:25][C:26]([F:29])([F:28])[F:27])[CH:20]=O.N1CCCCC1>C(Cl)(Cl)Cl>[OH:10][C:9]1[C:8]2[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=2[O:6][C:5](=[O:15])[C:4]=1[C:1](=[O:3])[CH:2]=[CH:20][C:19]1[CH:22]=[CH:23][C:24]([O:25][C:26]([F:27])([F:28])[F:29])=[C:17]([Cl:16])[CH:18]=1

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 27788913-Chloro-4-(trifluoromethoxy)benzaldehydeHCID 546774033-Acetyl-4-hydroxy-2H-chromen-2-one

생성물 1

HCID 76211114HCID 76211114, 화합물수율 36.2%

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A mixture of 2.25 g of 3-acetyl-4-hydroxy-2H-1-benzopyran-2-one, 2.25 g of 3-chloro-4-(trifluoromethoxy)benzaldehyde, 20 ml of chloroform and 0.7 ml of piperidine was heated under refluxing for 2 hours and 30 minutes. After cooled to room temperature, the reaction mixture was concentrated under reduced pressure, and the residue was subjected to column chromatography. Resulting crystals were washed with 40 ml of t-butyl methyl ether to obtain 1.49 g of 4-hydroxy-3-[3-[3-chloro-4-(trifluoromethoxy)phenyl]-1-oxo-2-propenyl]-2H-1-benzopyran-2-one [Compound No. (1c-6)] was obtained as a yellow crystal.

후처리

  1. temperaturewas heated
  2. temperatureunder refluxing for 2 hours and 30 minutes
  3. concentrationthe reaction mixture was concentrated under reduced pressure
  4. customResulting crystals
  5. washwere washed with 40 ml of t-butyl methyl ether

출처 및 근거

ORD 기록
ord-f556d4fe01f1480cb1a856a18b6c926a
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08524729B2

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