Water → 6-{[(6RS,7SR)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]oxy}pyridine-2-carboxylic acid

HRID 1022723노트

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HRID 1022723 반응식
[OH-].[Na+].[Cl:3][C:4]1[CH:5]=[C:6]([CH:11]2[O:17][CH2:16][CH2:15][N:14]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:13][CH:12]2[O:25][C:26]2[CH:31]=[CH:30][CH:29]=[C:28]([C:32]([O:34]C)=[O:33])[N:27]=2)[CH:7]=[CH:8][C:9]=1[Cl:10].O>C(O)C>[C:21]([O:20][C:18]([N:14]1[CH2:13][CH:12]([O:25][C:26]2[N:27]=[C:28]([C:32]([OH:34])=[O:33])[CH:29]=[CH:30][CH:31]=2)[CH:11]([C:6]2[CH:7]=[CH:8][C:9]([Cl:10])=[C:4]([Cl:3])[CH:5]=2)[O:17][CH2:16][CH2:15]1)=[O:19])([CH3:24])([CH3:22])[CH3:23]

참가 물질

5

반응물 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 66976194HCID 66976194, 화합물

생성물 1

HCID 669764066-{[(6RS,7SR)-4-(tert-butoxycarbonyl)-7-(3,4-dichlorophenyl)-1,4-oxazepan-6-yl]oxy}pyridine-2-carboxylic acid수율 33.8%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
70 °C

실험 절차

2M Aqueous sodium hydroxide solution (1.7 mL) was added to a solution of tert-butyl (6RS,7SR)-7-(3,4-dichlorophenyl)-6-{[6-(methoxycarbonyl)pyridin-2-yl]oxy}-1,4-oxazepane-4-carboxylate (210 mg) in ethanol (5 ml), and the mixture was stirred at room temperature overnight and at 70° C. for 2 hr. Water was added to the reaction mixture, and the mixture was washed with diethyl ether. The obtained aqueous layer was neutralized with 1 M hydrochloric acid, and the mixture was extracted with ethyl acetate. The obtained extract was washed with brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (69 mg).

후처리

  1. washthe mixture was washed with diethyl ether
  2. extractionthe mixture was extracted with ethyl acetate
  3. extractionThe obtained extract
  4. washwas washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-3a68a4cb0a7848aebf080baf94fa3f60
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722662B2

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