Sodium Acetate → HCID 14501368, 화합물

HRID 1904600노트

반응식

HRID 1904600 반응식
[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

참가 물질

4

반응물 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

생성물 1

HCID 14501368HCID 14501368, 화합물수율 62.1%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-32bc50d8004744f1b297e9f3a6ab2714
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839355

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