Sodium Acetate → HCID 14501361, 화합물

HRID 1904597노트

반응식

HRID 1904597 반응식
[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

참가 물질

4

반응물 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

생성물 1

HCID 14501361HCID 14501361, 화합물수율 51.8%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4f544419b7b4475cabbee7bf6f5bbe0a
출처 데이터셋
uspto-grants-1989_06
특허 번호
US04839355

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