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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
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2192945
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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Komponenten

4

Edukt 1

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

Produkt 1

HCID 44199002(2R)-2-[3-cyclopropyl-4-(cyclopropylsulfonyl)phenyl]-N-[5-(2-hydroxyethoxy)pyrazin-2-yl]-3-[(1R)-3-oxocyclopentyl]propanamideAusbeute 69,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 178418390HCID 178418390, VerbindungKatalysator
HCID 887
Methanol
Lösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  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)

Quellen und Nachweise

ORD-Eintrag
ord-8af8d3cc2a554b92a02ecb1b70c2ff80
Quelldatensatz
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08329707B2

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