StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrochloric Acid → HCID 57920068, Verbindung

HRID 19171
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 19171
CC1(C)[O:6][C@@H:5]([C:7]2[N:8]=[CH:9][C:10]([NH:13][C:14](=[O:38])[C@@H:15]([N:20]3[CH2:24][C:23]([O:25][C:26]4[C:31]([F:32])=[CH:30][CH:29]=[C:28]([O:33][CH2:34][CH3:35])[C:27]=4[F:36])=[CH:22][C:21]3=[O:37])[CH2:16][CH:17]([CH3:19])[CH3:18])=[N:11][CH:12]=2)[CH2:4][O:3]1.Cl>O1CCCC1.C(OCC)(=O)C>[OH:6][C@@H:5]([C:7]1[N:8]=[CH:9][C:10]([NH:13][C:14](=[O:38])[C@@H:15]([N:20]2[CH2:24][C:23]([O:25][C:26]3[C:31]([F:32])=[CH:30][CH:29]=[C:28]([O:33][CH2:34][CH3:35])[C:27]=3[F:36])=[CH:22][C:21]2=[O:37])[CH2:16][CH:17]([CH3:18])[CH3:19])=[N:11][CH:12]=1)[CH2:4][OH:3]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 57920045(S)-2-[4-(3-Ethoxy-2,6-difluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid [5-((S)-2,2-dimethyl-[1,3]dioxolan-4-yl)-pyrazin-2-yl]-amide

Produkt 1

HCID 57920068HCID 57920068, VerbindungAusbeute 90,1 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittel
HCID 8857
Ethyl Acetate
Lösungsmittel

Versuchsvorschrift

A solution of (S)-2-[4-(3-ethoxy-2,6-difluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid [5-((S)-2,2-dimethyl-[1,3]dioxolan-4-yl)-pyrazin-2-yl]-amide (prepared in Example 152, 0.251 g, 0.46 mmol) in tetrahydrofuran (25 mL) was treated with 1N aqueous hydrochloric acid (10 mL). The reaction mixture was stirred for 20 h at room temperature. The reaction mixture was diluted with ethyl acetate, washed with saturated sodium bicarbonate, a saturated sodium chloride solution and dried over magnesium sulfate. The mixture was filtered and evaporated and the residue purified by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 12 g; 10% to 100% (9:1 dichloromethane:methanol)/hexanes) to afford (S)-2-[4-(3-ethoxy-2,6-difluoro-phenoxy)-2-oxo-2,5-dihydro-pyrrol-1-yl]-4-methyl-pentanoic acid [5-((S)-1,2-dihydroxy-ethyl)-pyrazin-2-yl]-amide (0.210 g, 90%) as a fluffy white solid: HR-ES-MS m/z calculated for C24H28F2N4O6, [M+H]+ 507.2050 observed 507.2051; 1H NMR (300 MHz, DMSO-d6) δ ppm 0.92 (d, J=6.9 Hz, 3H), 0.95 (d, J=6.9 Hz, 3H), 1.35 (t, J=6.9 Hz, 3H), 1.40-1.56 (m, 1H), 1.56-1.73 (m, 1H), 1.75-1.93 (m, 1H), 3.42-3.62 (m, 1H), 3.61-3.74 (m, 1H), 4.13 (q, J=6.9 Hz, 2H), 4.31 (d, J=18.7 Hz, 1H), 4.51-4.69 (m, 2H), 4.73 (t, J=5.7 Hz, 1H). 5.02 (dd, J=10.6, 4.2 Hz, 1H), 5.08 (s, 1H), 5.55 (d, J=5.1 Hz, 1H), 7.12-7.23 (m, 1H), 7.23-7.33 (m, 1H), 8.45 (s, 1H), 9.17 (s, 1H), 11.16 (s, 1H).

Aufarbeitung

  1. washwashed with saturated sodium bicarbonate
  2. dry with materiala saturated sodium chloride solution and dried over magnesium sulfate
  3. filtrationThe mixture was filtered
  4. customevaporated
  5. customthe residue purified by ISCO flash chromatography (Teledyne Isco RediSep Flash Column 12 g; 10% to 100% (9:1 dichloromethane:methanol)/hexanes)

Quellen und Nachweise

ORD-Eintrag
ord-0b46d87d218640dfb9dc6ce382576673
Quelldatensatz
uspto-grants-2010_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07741327B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion