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Trifluoroacetic acid water → Methyl 3-(4-aminopiperidin-1-yl)benzoate

HRID 43825
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HRID 43825 반응식
C(OC([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:19]=[C:20]([CH:25]=[CH:26][CH:27]=2)[C:21]([O:23][CH3:24])=[O:22])[CH2:14][CH2:13]1)=O)C1C=CC=CC=1.O.C(O)(C(F)(F)F)=O>O1CCCC1.CO.[C].[Pd]>[NH2:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[CH:19]=[C:20]([CH:25]=[CH:26][CH:27]=2)[C:21]([O:23][CH3:24])=[O:22])[CH2:14][CH2:13]1
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참가 물질

5

반응물 2

HCID 22392675Trifluoroacetic acid waterHCID 68405998Methyl 3-(4-benzyloxycarbonylaminopiperidin-1-yl)benzoate

생성물 1

HCID 67339058Methyl 3-(4-aminopiperidin-1-yl)benzoate

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

10% palladium-carbon (wet, 200 mg) was added to a mixed solution of methyl 3-(4-benzyloxycarbonylaminopiperidin-1-yl)benzoate obtained in Example (192c) (120 mg, 0.345 mmol) in tetrahydrofuran/methanol=1/1 (10 mL), and the mixture was catalytically hydrogenated at room temperature for three hours. The catalyst was filtered off, and the filtrate was evaporated under reduced pressure to obtain methyl 3-(4-aminopiperidin-1-yl)benzoate as a colorless oily substance. The resulting amine was dissolved in a mixed solution of N,N-dimethylacetamide/dichloromethane=1/1 (8 mL). 4-Chloro-5-ethyl-1H-imidazole-2-carboxylic acid (described in Example 1d, 190 mg, 1.1 mmol), 1-hydroxybenzotriazole (220 mg, 1.63 mmol), 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide hydrochloride (312 mg, 1.63 mmol) and triethylamine (227 μL, 1.63 mmol) were added, and the mixture was stirred at room temperature overnight. The reaction solution was diluted with ethyl acetate, washed with brine, and then dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (elution solvent: hexane/ethyl acetate=1/1) to obtain 88 mg of the title compound as a colorless solid (41%).

후처리

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-19f6236aaa8e41fc98fdf3a031afbd43
출처 데이터셋
uspto-grants-2013_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08536197B2

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