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Hydrochloric Acid → HCID 22901902, Verbindung

HRID 1735989
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1735989
C(OC([O:6][CH:7]1[C:12]2[CH:13]=[C:14]([S:16]([NH:19][C:20]([CH3:23])([CH3:22])[CH3:21])(=[O:18])=[O:17])[S:15][C:11]=2[S:10](=[O:25])(=[O:24])[N:9](C(OCC)C)[CH2:8]1)C)C.Cl>C1COCC1>[OH:6][CH:7]1[C:12]2[CH:13]=[C:14]([S:16]([NH:19][C:20]([CH3:21])([CH3:22])[CH3:23])(=[O:17])=[O:18])[S:15][C:11]=2[S:10](=[O:25])(=[O:24])[NH:9][CH2:8]1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 19434048HCID 19434048, Verbindung

Produkt 1

HCID 22901902HCID 22901902, VerbindungAusbeute 75 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of the product from Step E (158 g, 0.325 mol), THF (700 mL) and 2N HCl (180 mL) were stirred at room temperature for 20 hr. After evaporating the THF, the aqueous mixture was cooled to 0° C. and sodium bicarbonate (50 g) was carefully added followed by water (400 mL) and ethyl acetate (500 mL). The two layers were separated and the aqueous layer was extracted with ethyl acetate (250 mL). The combined organic extracts were washed with brine, dried (MgSO4) and evaporated to give a foam which was triturated with methylene chloride (200 mL) to give a solid (81.7 g, 75%): mp 144°-147° C. Recrystallization of this solid from methylene chloride gave an off-white solid: mp 163°-165° C.

Aufarbeitung

  1. customAfter evaporating the THF
  2. temperaturethe aqueous mixture was cooled to 0° C.
  3. additionsodium bicarbonate (50 g) was carefully added
  4. customThe two layers were separated
  5. extractionthe aqueous layer was extracted with ethyl acetate (250 mL)
  6. washThe combined organic extracts were washed with brine
  7. dry with materialdried (MgSO4)
  8. customevaporated
  9. customto give a foam which
  10. customwas triturated with methylene chloride (200 mL)

Quellen und Nachweise

ORD-Eintrag
ord-f13e86aa1547499ea35d5ee6ccdd715c
Quelldatensatz
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05538966

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