Sodium Acetate → HCID 14501361、化合物

HRID 1904597ノート

反応式

HRID 1904597 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[C:9]([F:29])=[C:10]([F:28])[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]([CH3:30])[N:3]=1.C([O-])(=O)C.[Na+]>Cl>[CH3:30][C:4]1[CH:5]=[C:6]([C:8]2[C:9]([F:29])=[C:10]([F:28])[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 14501359ethyl (S)-10-(2,6-dimethyl-4-pyridinyl)-8,9-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate

生成物 1

HCID 14501361HCID 14501361、化合物収率 51.8%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 1.20 g ethyl (S)-10-(2,6-dimethyl-4-pyridinyl)-8,9-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylate in 15 ml 1M hydrochloric acid was heated at reflux for 2 hours. The reaction mixture was cooled, poured into sodium acetate solution and extracted with methylene dichloride. The extract was dried (sodium sulfate) and concentrated, and the residue was crystallized from methanol to give 0.58 g (S)-10-(2,6-dimethyl-4-pyridinyl)-8,9-difluoro-3-methyl-7-oxo-2,3-dihydro-7H-pyrido[1,2,3-de][1,4]benzoxazine-6-carboxylic acid as a colorless solid, m.p. 307°-310° C., [α]D25 =-39.1° (1% in chloroform).

後処理

  1. temperatureat reflux for 2 hours
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with methylene dichloride
  4. dry with materialThe extract was dried (sodium sulfate)
  5. concentrationconcentrated
  6. customthe residue was crystallized from methanol

出典と根拠

ORDレコード
ord-4f544419b7b4475cabbee7bf6f5bbe0a
出典データセット
uspto-grants-1989_06
特許番号
US04839355

反応ノート

読み込み中…