b) Microbiological Reduction Of the dried biomass 0,5g were suspended in 100cm³ of YNB(containing 2g D-glucose). To the suspension was added a
solution of 50mg of 3,4,5-Trimethoxy-ß-nitrostyrene in 10cm³ DMSO and the reaction mixture was under anaerobic conditions heated to 60°C for 24h.
The insoluble part was centrifuged(15min;1500g) off, the sediment was washed through with a mixture of 1-propanol+ammonia(4:1)(2x50cm³). Supernatant
of the residue was extracted with Et2O(3x65cm³) and finally the combined ether as well as the 1-propanol+ammonia extracts werde distilled to dryness.
The residue was dissolved into 5cm³ of a mixture of ethyl acetate +pyridine +acetic acid +water(ratio of 5:5:1:3) and the so obtained solution was
fractionated on a cellulose column(60x5cm) under utilisation of the same mixture. Of this where 5cm³ of the eluent taken, in which for the presence
of an amino group was checked according for [12]. The combined eluent were evaporated using an aspirator vacuum, the remains of solvent again removed
using water(3x5cm³), on which the desired mescaline(22mg, 52%), with a melting point of(HCl; MeOH/AcOEt = 182°C);(Picrate; H2O = 222°C) was
obtained. |
