Hydrochloric Acid → 6-(1-((Tert-butoxy)carbonyl)piperidin-4-yl)pyridine-3-carboxylic acid

HRID 1427048노트

반응식

HRID 1427048 반응식
[OH-].[Na+].[C:3]([O:7][C:8]([N:10]1[CH2:15][CH2:14][CH:13]([C:16]2[CH:25]=[CH:24][C:19]([C:20]([O:22]C)=[O:21])=[CH:18][N:17]=2)[CH2:12][CH2:11]1)=[O:9])([CH3:6])([CH3:5])[CH3:4].Cl>C(O)C>[C:3]([O:7][C:8]([N:10]1[CH2:11][CH2:12][CH:13]([C:16]2[CH:25]=[CH:24][C:19]([C:20]([OH:22])=[O:21])=[CH:18][N:17]=2)[CH2:14][CH2:15]1)=[O:9])([CH3:6])([CH3:4])[CH3:5]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86730350Methyl 6-(1-(tert-butoxycarbonyl)piperidin-4-yl)nicotinate

생성물 1

HCID 867303496-(1-((Tert-butoxy)carbonyl)piperidin-4-yl)pyridine-3-carboxylic acid수율 52%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A 2 M sodium hydroxide solution (20 mL) was added to a solution of methyl 6-(1-(tert-butoxycarbonyl)piperidin-4-yl)nicotinate described in Production Example 28-2 (1.07 g, 3.32 mmol) in ethanol (5 mL), and the mixture was stirred for 1 hour. 2 M hydrochloric acid was added to the reaction liquid at 0° C. The aqueous layer was extracted with ethyl acetate. The combined organic layer was washed with a saturated saline solution and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration and then the filtrate was concentrated under vacuum to obtain the title compound (534 mg, 52%).

후처리

  1. extractionThe aqueous layer was extracted with ethyl acetate
  2. washThe combined organic layer was washed with a saturated saline solution
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe drying agent was separated by filtration
  5. concentrationthe filtrate was concentrated under vacuum

출처 및 근거

ORD 기록
ord-4f2dfd6fb92c4eea90ae5c4f177f9485
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08933099B2

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