2,8-Dimethyl-3-methylene-1-oxa-8-azaspiro(4,5)decane → 147816-26-0

HRID 1653830

Reaktionsgleichung

Reaktionsgleichung von HRID 1653830
[CH3:1][CH:2]1[C:6](=[CH2:7])[CH2:5][C:4]2([CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)[O:3]1.[C:14]([OH:23])(=[O:22])[C@@H:15]([C@H:17]([C:19]([OH:21])=[O:20])[OH:18])[OH:16]>C(O)C>[OH2:3].[C:19]([C@@H:17]([C@H:15]([C:14]([OH:23])=[O:22])[OH:16])[OH:18])([OH:21])=[O:20].[CH3:1][C@H:2]1[C:6](=[CH2:7])[CH2:5][C:4]2([CH2:12][CH2:11][N:10]([CH3:13])[CH2:9][CH2:8]2)[O:3]1

Komponenten

4

Edukt 2

HCID 1772332,8-Dimethyl-3-methylene-1-oxa-8-azaspiro(4,5)decaneHCID 444305L-Tartaric acid

Produkt 1

HCID 6918121147816-26-0Ausbeute 47,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To 90% aqueous ethanol (water:ethanol =1:9, v/v), 7 g of (±)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane and 5.79 g of L-tartaric acid were added and dissolved by heating at 60° C. The resulting solution was allowed to cool and maintained at about 4° C. for 15 hours. The resulting crystals were collected by filtration and, without drying, recrystallized from 9 ml of 90% aqueous ethanol. This recrystallization procedure was repeated further twice and the crystals obtained were dried under reduced pressure to give 3.22 g of (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate.

Aufarbeitung

  1. dissolutiondissolved
  2. temperatureto cool
  3. temperaturemaintained at about 4° C. for 15 hours
  4. filtrationThe resulting crystals were collected by filtration
  5. customwithout drying
  6. customrecrystallized from 9 ml of 90% aqueous ethanol
  7. customThis recrystallization procedure
  8. customthe crystals obtained
  9. customwere dried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cf37951cbf1c4a4992494c9e6c17d2eb
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05403931

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