Piperidine → 6,7-Difluoroquinazolin-4(3H)-one

HRID 353159

반응식

HRID 353159 반응식
[NH2:1][C:2]1[CH:10]=[C:9]([F:11])[C:8]([F:12])=[CH:7][C:3]=1[C:4](O)=[O:5].[NH:13]1CCCC[CH2:14]1.N1C=NC=NC=1>C(O)C>[F:12][C:8]1[CH:7]=[C:3]2[C:2](=[CH:10][C:9]=1[F:11])[N:1]=[CH:14][NH:13][C:4]2=[O:5]

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 92621,3,5-TriazineHCID 7359652-Amino-4,5-difluorobenzoic acid

생성물 1

HCID 1354713086,7-Difluoroquinazolin-4(3H)-one수율 86%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 4.81 g (27.8 mmol) of commercially available 2-amino-4,5-difluorobenzoic acid in 20 ml of ethanol were added 1.92 ml (19.4 mmol) of piperidine and 2.25 g (27.8 mmol) of 1,3,5-triazine, followed by heating under reflux in an atmosphere of argon for 6.5 hours. After the reaction mixture was allowed to cool to room temperature, the solvent was evaporated. To the residue was added water, and the resulting mixture was neutralized with 4 N hydrochloric acid. The precipitated crystals were collected by filtration, washed with water, and dried to give 4.37 g (86%) of 6,7-difluoro-4(3H)-quinazolone.

후처리

  1. temperatureby heating
  2. temperatureunder reflux in an atmosphere of argon for 6.5 hours
  3. customthe solvent was evaporated
  4. additionTo the residue was added water
  5. filtrationThe precipitated crystals were collected by filtration
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-26367b7bf5f44bffb86b8d2214bf5dda
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06750218B2

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