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Water → 6-[3-Cyclopentyl-2-(4-nitro-phenyl)-propionylamino]-nicotinic acid

HRID 2296960
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HRID 2296960 반응식
C[O:2][C:3](=[O:35])[C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:34])[CH:12]([C:19]2[CH:24]=[CH:23][C:22]([NH:25]C(C3C=NC=CC=3)=O)=[CH:21][CH:20]=2)[CH2:13][CH:14]2[CH2:18][CH2:17][CH2:16][CH2:15]2)=[N:6][CH:5]=1.[OH-:36].[Li+].[OH2:38]>O1CCCC1>[CH:14]1([CH2:13][CH:12]([C:19]2[CH:24]=[CH:23][C:22]([N+:25]([O-:38])=[O:36])=[CH:21][CH:20]=2)[C:11]([NH:10][C:7]2[CH:8]=[CH:9][C:4]([C:3]([OH:2])=[O:35])=[CH:5][N:6]=2)=[O:34])[CH2:18][CH2:17][CH2:16][CH2:15]1
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참가 물질

5

반응물 3

HCID 962WaterHCID 3939Lithium HydroxideHCID 102055406-(3-Cyclopentyl-2-{4-[(pyridine-3-carbonyl)-amino]-phenyl}-propionylamino)-nicotinic acid methyl ester

생성물 1

HCID 223150786-[3-Cyclopentyl-2-(4-nitro-phenyl)-propionylamino]-nicotinic acid수율 7.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
25 °C

실험 절차

A solution of 6-(3-cyclopentyl-2-{4-[(pyridine-3-carbonyl)-amino]-phenyl}-propionylamino)-nicotinic acid methyl ester (prepared in Example 16, 87.2 mg, 0.18 mmol) in tetrahydrofuran (8 mL) and water (2 mL) was treated with lithium hydroxide (17.0 mg, 0.41 mmol). The reaction was stirred at 25° C. for 20 h. At this time, the reaction was concentrated in vacuo. The residue was diluted with water (25 mL) and extracted with diethyl ether (1×20 mL). The aqueous layer was acidified to pH=1 with a 3N aqueous hydrochloric acid solution and was extracted with methylene chloride (3×50 mL). The combined organic extracts were washed with water (1×50 mL) and a saturated aqueous sodium chloride solution (2×50 mL), dried over magnesium sulfate, filtered, and concentrated in vacuo. High pressure liquid chromatography (Chromegasphere SI-60, 10 μM, 60 Å, 25 cm×23 cm ID, 100% ethyl acetate with acetic acid) afforded 6-[3-cyclopentyl-2-(4-nitro-phenyl)-propionylamino]-nicotinic acid (6.4 mg, 7.5%) as a pale yellow oil: EI-HRMS m/e calcd for C16H26N4O4 (M+) 458.1954, found 458.1967.

후처리

  1. concentrationAt this time, the reaction was concentrated in vacuo
  2. additionThe residue was diluted with water (25 mL)
  3. extractionextracted with diethyl ether (1×20 mL)
  4. extractionwas extracted with methylene chloride (3×50 mL)
  5. washThe combined organic extracts were washed with water (1×50 mL)
  6. dry with materiala saturated aqueous sodium chloride solution (2×50 mL), dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-0885a0fd202342c1a6366d99e136b08b
출처 데이터셋
uspto-grants-2002_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06489485B2

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