Sodium Acetate → HCID 14501368、化合物

HRID 1904600ノート

反応式

HRID 1904600 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[C:9]([F:28])=[CH:10][C:11]3[C:21](=[O:22])[C:20]([C:23]([O:25]CC)=[O:24])=[CH:19][N:13]4[C@@H:14]([CH3:18])[CH2:15][O:16][C:17]=2[C:12]=34)[CH:5]=[C:4]([CH3:29])[N:3]=1.C([O-])(=O)C.[Na+]>Cl>[CH3:29][C:4]1[CH:5]=[C:6]([C:8]2[C:9]([F:28])=[CH:10][C:11]3[C:21](=[O:22])[C:20]([C:23]([OH:25])=[O:24])=[CH:19][N:13]4[C@@H:14]([CH3:18])[CH2:15][O:16][C:17]=2[C:12]=34)[CH:7]=[C:2]([CH3:1])[N:3]=1

参加物

4

反応物 2

HCID 517045Sodium AcetateHCID 14501365ethyl (S)-10-(2,6-dimethyl-4-pyridinyl)-9-fluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate

生成物 1

HCID 14501368HCID 14501368、化合物収率 62.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A mixture of 0.52 g ethyl (S)-10-(2,6-dimethyl-4-pyridinyl)-9-fluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate and 10 ml 1M hydrochloric acid was heated at reflux for one hour. The reaction mixture was cooled, poured into sodium acetate solution and extracted with chloroform. The extract was dried (sodium sulfate) and concentrated, and the residue was recrystallized from methanol to give 300 mg (S)-10-(2,6-dimethyl-4-pyridinyl)-9-fluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid, colorless powder, m.p. 305°-308° C., [α]D25 =-39.8°.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for one hour
  3. temperatureThe reaction mixture was cooled
  4. extractionextracted with chloroform
  5. dry with materialThe extract was dried (sodium sulfate)
  6. concentrationconcentrated
  7. customthe residue was recrystallized from methanol

出典と根拠

ORDレコード
ord-32bc50d8004744f1b297e9f3a6ab2714
出典データセット
uspto-grants-1989_06
特許番号
US04839355

反応ノート

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