Reaktionsgleichung
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11](=[O:13])[CH3:12])=[CH:4][C:3]=2[O:2]1.P(O)([O-])([O-])=O.[Na+].[Na+].P(=O)(O)(O)O.O=C[C@@H]([C@H]([C@@H]([C@@H](CO)O)O)O)O>O>[CH3:12][C@H:11]([OH:13])[CH2:10][C:5]1[CH:6]=[CH:7][C:8]2[O:9][CH2:1][O:2][C:3]=2[CH:4]=1Komponenten
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
1 equiv. of 3,4-methylenedioxyphenyl acetone, 0.45 equiv. disodium phosphate, 0.03 equiv. phosphoric acid, 12.5 volumes AD-7 resin and 5.8 volumes of water were mixed together and stirred for 15-60 minutes at 20°-25° C. 2.27 equiv. of glucose were added and Z. rouxii ATCC 14462 is added in an amount of 1.5 grams wet cell paste per gram of ketone (this is 0.375 grams/gram on a dry basis). This mixture was diluted with water to 25 volumes and then gently stirred at 33°-35° C. for 8-16 hours. The mixture was filtered on a 100 mesh (~150 micron) stainless steel screen, and the resin which was retained by the screen was washed with 25 volumes of water split into 4 separate portions. The product, which was adsorbed to the resin, was then desorbed from the resin with 25 volumes of acetone. The acetone/product solution was then stripped to dryness under vacuum to yield the title intermediate as a yellow, medium viscosity oil. The in-situ yield was 97-100%, while the isolated yield was 85-90%. The potency was 80-95% and the EE is 100%.
Aufarbeitung
- stirringgently stirred at 33°-35° C. for 8-16 hours
- filtrationThe mixture was filtered on a 100 mesh (~150 micron) stainless steel screen
- washwas washed with 25 volumes of water
- customsplit into 4
- customseparate portions
Quellen und Nachweise
- ORD-Eintrag
- ord-35e07c4d51164e26ad4830a3d3e764b0
- Quelldatensatz
- uspto-grants-1997_09
- Patentnummer
- US05665878
Verknüpfte Notizen
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