L-Tartaric acid → (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate

HRID 1653831Notizen

Reaktionsgleichung

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

Komponenten

Reaktionsbedingungen

Temperatur: 65 °C

Versuchsvorschrift

To 28 l of 90% aqueous ethanol (water:ethanol =1:9, v/v), 7.74 kg of L-tartaric acid was added and dissolved by heating at 65° C. To the resulting solution was added 9.41 kg of (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8azaspiro[4.5]decane dropwise. The mixture was allowed to cool and maintained for crystallization at 0° C. for 15 hours. The resulting crystals were collected by filtration and dried under reduced pressure to give 14.76 kg of (-)-(S)-2,8-dimethyl-3-methylene-1-oxa-8-azaspiro[4.5]decane L-tartrate monohydrate. The physicochemical properties of this compound were in agreement with those of the compound obtained in Example 1.

Aufarbeitung

dissolutiondissolved
temperatureto cool
temperaturemaintained for crystallization at 0° C. for 15 hours
filtrationThe resulting crystals were collected by filtration
customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag: ord-8832e1eaccea4b7b8650ad97c9844f74
Quelldatensatz: uspto-grants-1995_04
DOI: 10.6084/m9.figshare.5104873.v1
Patentnummer: US05403931

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