Potassium Carbonate → HCID 66975246, 화합물

HRID 1022637노트

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HRID 1022637 반응식
[OH:1][C:2]1[C:7]([C:8]([O:10][CH3:11])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].[Cl:18][C:19]1[CH:24]=[CH:23][C:22]([C@@H:25]2[O:31][CH2:30][CH2:29][N:28]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:27][C@H:26]2[CH2:39]OS(C)(=O)=O)=[CH:21][C:20]=1[F:45]>COCCOC>[Cl:18][C:19]1[CH:24]=[CH:23][C:22]([C@@H:25]2[O:31][CH2:30][CH2:29][N:28]([C:32]([O:34][C:35]([CH3:37])([CH3:36])[CH3:38])=[O:33])[CH2:27][C@H:26]2[CH2:39][N:3]2[CH:4]=[CH:5][CH:6]=[C:7]([C:8]([O:10][CH3:11])=[O:9])[C:2]2=[O:1])=[CH:21][C:20]=1[F:45]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 86663855tert-butyl (6S,7R)-7-(4-chloro-3-fluorophenyl)-6-{[(methylsulfonyl)oxy]methyl}-1,4-oxazepane-4-carboxylateHCID 178498115HCID 178498115, 화합물

생성물 1

HCID 66975246HCID 66975246, 화합물수율 72.2%

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

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온도
80 °C

실험 절차

Methyl 2-hydroxypyridine-3-carboxylate (1.48 g) and potassium carbonate (2.23 g) were added to a solution of tert-butyl (6S,7R)-7-(4-chloro-3-fluorophenyl)-6-{[(methylsulfonyl)oxy]methyl}-1,4-oxazepane-4-carboxylate (3.53 g) in 1,2-dimethoxyethane (70 ml). The reaction mixture was stirred at 80° C. overnight. The reaction mixture was concentrated under reduced pressure, water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography to give the title compound (2.88 g).

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, water
  2. additionwas added to the residue
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-cdea681f59954f00b8ada60d92b0abe1
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722662B2

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