Hydrochloric Acid → HCID 22857049, Verbindung

HRID 2211410Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2211410
[C:1]1([C:7]2([C:32]3[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=3)[C@@H:15]3[C@@H:11]([CH2:12][N:13](C(OC(C)(C)C)=O)[CH2:14]3)[C@@:10]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[O:30][CH3:31])(O)[CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[ClH:38]>C(O)(=O)C>[ClH:38].[C:32]1([C:7]2([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:8][CH:9]=[C:10]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][C:25]=3[O:30][CH3:31])[C@H:11]3[C@@H:15]2[CH2:14][NH:13][CH2:12]3)[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 22857048HCID 22857048, Verbindung

Produkt 1

HCID 22857049HCID 22857049, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution of 8.56 g of (3aS,4S,7aS)-7,7-diphenyl-4-(2-methoxyphenyl)-2-tert-butoxycarbonyl-perhydroisoindol-4-ol in 53 cm3 of acetic acid and 30 cm3 of 12N hydrochloric acid is heated at 95° C. for 45 minutes, and then cooled to room temperature and concentrated to dryness under reduced pressure (2.7 kPa). The residue is recrystallised from 20 cm3 of acetonitrile. 5.2 g of (3aS,7aR)-4,4-diphenyl-7-(2-methoxyphenyl)-2,3,3a, 4,5,7a-hexahydroisoindole hydrochloride are obtained in the form of white crystals which melt at a temperature above 300° C., and the product is used in the crude state in the subsequent syntheses.

Aufarbeitung

  1. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
  2. customThe residue is recrystallised from 20 cm3 of acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-2f900bf2c8484294ac0ea55502ed1e00
Quelldatensatz
uspto-grants-1995_10
Patentnummer
US05463077

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