Piperidine → HCID 76211114、化合物

HRID 38301

反応式

HRID 38301 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 76211114HCID 76211114、化合物収率 36.2%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f556d4fe01f1480cb1a856a18b6c926a
出典データセット
uspto-grants-2013_09
特許番号
US08524729B2

関連ノート

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