Hydrochloric Acid → HCID 67916022, Verbindung

HRID 1029944Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1029944
[Cl:1][C:2]1[CH:3]=[C:4]([C:8]2([C:23]3[CH:28]=[CH:27][CH:26]=[C:25]([Cl:29])[CH:24]=3)[CH:16]3[CH:12]([CH2:13][N:14](C(OC=C)=O)[CH2:15]3)[C:11](=[O:22])[CH2:10][CH2:9]2)[CH:5]=[CH:6][CH:7]=1.Cl>O1CCOCC1.C(OC(C)C)(C)C>[ClH:1].[Cl:29][C:25]1[CH:24]=[C:23]([C:8]2([C:4]3[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[CH:3]=3)[CH:16]3[CH:12]([CH2:13][NH:14][CH2:15]3)[C:11](=[O:22])[CH2:10][CH2:9]2)[CH:28]=[CH:27][CH:26]=1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 67915885(3aRS,7aRS)-7,7-bis(3-chlorophenyl)-2-vinyloxycarbonylperhydro-4-isoindolone

Produkt 1

HCID 67916022HCID 67916022, VerbindungAusbeute 144,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 7914Diisopropyl EtherLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

(3aRS,7aRS)-7,7-bis-(3-chlorophenyl)-2-vinyloxycarbonyl-4-perhydroisoindolone (1.5 g) is treated with a 6N solution (7.4 cc) of hydrochloric acid in dioxane for 2 hours at 25° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the residue is heated for 1 hour in solution in ethanol at 60° C. and then stirred for 6 hours at 25° C. The solution is concentrated to dryness under reduced pressure (2.7 kPa) and the meringue obtained is solidified in isopropyl ether. The precipitate is drained and washed with isopropyl ether and then dried to give 7,7-bis-(3-chlorophenyl)-4-perhydroisoindolone hydrochloride (1 g).

Aufarbeitung

  1. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
  2. concentrationThe solution is concentrated to dryness under reduced pressure (2.7 kPa)
  3. customthe meringue obtained
  4. washwashed with isopropyl ether
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-df257deec7c846ceacddc2f1551cf0d4
Quelldatensatz
uspto-grants-1992_04
Patentnummer
US05102667

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