Hydrochloric Acid → HCID 67736902, Verbindung

HRID 2211408Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2211408
[ClH:1].[C:2]1([C:8]2([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[C@@H:16]3[C@@H:12]([CH2:13][N:14](C(OC(C)(C)C)=O)[CH2:15]3)[C@:11]([F:32])([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[O:30][CH3:31])[CH2:10][CH2:9]2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>O1CCOCC1>[ClH:1].[C:33]1([C:8]2([C:2]3[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=3)[C@@H:16]3[C@@H:12]([CH2:13][NH:14][CH2:15]3)[C@:11]([F:32])([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[O:30][CH3:31])[CH2:10][CH2:9]2)[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 57167112HCID 57167112, Verbindung

Produkt 1

HCID 67736902HCID 67736902, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel2×

Versuchsvorschrift

A solution of 6.3N hydrochloric acid in 20 cm3 of dioxane is added to a solution of 2.07 g of (3aS,4S,7aS)-7,7-diphenyl-4-fluoro-4-(2-methoxyphenyl)-2-tert-butoxycarbonyl-perhydroisoindole in 20 cm3 of dioxane at room temperature. The reaction mixture is stirred at this temperature for 3 hours and then concentrated to dryness under reduced pressure (2.7 kPa). The residue is crystallised in 40 cm3 of absolute ethanol and the crystals are filtered off and then dried. 1 g of (3aS,4S,7aS)-7,7-diphenyl-4-fluoro-4-(2-methoxyphenyl)-perhydroisoindole hydrochloride is obtained in the form of white crystals which melt at 270° C.

Aufarbeitung

  1. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  2. customThe residue is crystallised in 40 cm3 of absolute ethanol
  3. filtrationthe crystals are filtered off
  4. customdried

Quellen und Nachweise

ORD-Eintrag
ord-c54366de8ab14a95bfabf28aeba768e7
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05463077

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