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

HRID 353159

反応式

HRID 353159 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-26367b7bf5f44bffb86b8d2214bf5dda
出典データセット
uspto-grants-2004_06
特許番号
US06750218B2

関連ノート

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