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(2R)-N-{5-[2-(benzyloxy)ethoxy]pyrazin-2-yl}-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-3-[(1R)-3-oxocyclopentyl]propanamide → (2R)-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-N-[5-(2-hydroxyethoxy)pyrazin-2-yl]-3-[(1R)-3-oxocyclopentyl]propanamide

HRID 2192945
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HRID 2192945 반응식
C([O:8][CH2:9][CH2:10][O:11][C:12]1[N:13]=[CH:14][C:15]([NH:18][C:19](=[O:43])[C@@H:20]([C:28]2[CH:33]=[CH:32][C:31]([S:34]([CH:37]3[CH2:39][CH2:38]3)(=[O:36])=[O:35])=[C:30]([CH:40]3[CH2:42][CH2:41]3)[CH:29]=2)[CH2:21][C@H:22]2[CH2:26][CH2:25][C:24](=[O:27])[CH2:23]2)=[N:16][CH:17]=1)C1C=CC=CC=1>CO.[C].[Pd]>[CH:40]1([C:30]2[CH:29]=[C:28]([C@@H:20]([CH2:21][C@H:22]3[CH2:26][CH2:25][C:24](=[O:27])[CH2:23]3)[C:19]([NH:18][C:15]3[CH:14]=[N:13][C:12]([O:11][CH2:10][CH2:9][OH:8])=[CH:17][N:16]=3)=[O:43])[CH:33]=[CH:32][C:31]=2[S:34]([CH:37]2[CH2:39][CH2:38]2)(=[O:36])=[O:35])[CH2:42][CH2:41]1
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참가 물질

4

반응물 1

HCID 68670548(2R)-N-{5-[2-(benzyloxy)ethoxy]pyrazin-2-yl}-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-3-[(1R)-3-oxocyclopentyl]propanamide

생성물 1

HCID 44199002(2R)-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-N-[5-(2-hydroxyethoxy)pyrazin-2-yl]-3-[(1R)-3-oxocyclopentyl]propanamide수율 69.2%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 887Methanol용매

실험 절차

To a solution of (2R)-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-3-[(1R)-3-oxocyclopentyl]propionic acid (120 mg) in dichloromethane (5 mL) was sequentially added a solution of 0.5 M oxalyl chloride in dichloromethane (0.77 mL) and DMF (10 μL) under ice-cooling, followed by stirring under ice-cooling for 1 hour. Thereafter, 5-[2-(benzyloxy)ethoxy]pyrazin-2-amine (86 mg) and pyridine (0.05 mL) were added thereto under ice-cooling, followed by stirring for 2 hours under ice-cooling. To the reaction mixture was added water under ice-cooling, followed by extraction with ethyl acetate. The organic layer was sequentially washed with 1 M hydrochloric acid, saturated aqueous sodium bicarbonate, and saturated brine, and then dried over anhydrous magnesium sulfate. The oily substance obtained by concentration was purified by silica gel column chromatography (hexane:ethyl acetate=5:1-1:1) to obtain (2R)—N-{5-[2-(benzyloxy)ethoxy]pyrazin-2-yl}-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-3-[(1R)-3-oxocyclopentyl]propanamide (175 mg) as a pale yellow amorphous substance. To a solution of the obtained (2R)—N-{5-[2-(benzyloxy)ethoxy]pyrazin-2-yl}-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-3-[(1R)-3-oxocyclopentyl]propanamide (175 mg) in methanol (10 mL) was added 10% palladium carbon (50 mg). Under a hydrogen atmosphere, it was stirred at room temperature at 4 atm for 7 hours. The reaction mixture was filtered through Celite and concentrated. To a solution of the obtained oily substance in THF (10 mL) was added 1 M hydrochloric acid (10 mL) at room temperature, followed by stirring at room temperature for 30 minutes. The reaction mixture was extracted with ethyl acetate. The organic layer was sequentially washed with saturated aqueous sodium bicarbonate and saturated brine, and dried over anhydrous magnesium sulfate. The oily substance obtained by concentration was purified by silica gel column chromatography (wetting with hexane:ethyl acetate=1:1, chloroform:methanol=1:0-10:1) to obtain (2R)-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-N-[5-(2-hydroxyethoxy)pyrazin-2-yl]-3-[(1R)-3-oxocyclopentyl]propanamide (103 mg) as a pale yellow amorphous substance.

후처리

  1. filtrationThe reaction mixture was filtered through Celite
  2. concentrationconcentrated
  3. additionTo a solution of the obtained oily substance in THF (10 mL) was added 1 M hydrochloric acid (10 mL) at room temperature
  4. stirringby stirring at room temperature for 30 minutes
  5. extractionThe reaction mixture was extracted with ethyl acetate
  6. washThe organic layer was sequentially washed with saturated aqueous sodium bicarbonate and saturated brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. customThe oily substance obtained by concentration
  9. customwas purified by silica gel column chromatography (wetting with hexane:ethyl acetate=1:1, chloroform:methanol=1:0-10:1)

출처 및 근거

ORD 기록
ord-8af8d3cc2a554b92a02ecb1b70c2ff80
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08329707B2

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