Triethylamine → Deoxynojirimycin

温度

50 °C

50 g (0.23 mol) of 6-amino-6-desoxy-L-sorbose hydrochloride were dissolved in 500 ml of distilled water, and the solution was added in the course of one hour to a solution of 11.2 g of dimethylaminoborane in 500 ml of distilled water, whilst stirring at a temperature of 50° C. The mixture was stirred for one hour at room temperature and one hour at 50° C., 5 ml of triethylamine were added to it, and it was then poured over a column containing 800 ml of strongly basic ion exchanger ("Lewatit" MP 500 OH- -form). The exchanger was washed with distilled water, and the runnings collected were concentrated to a syrup on a rotary evaporator. The concentrated syrup was crystallised at 50° C., with addition of a large amount of ethanol. The suspension of crystals was cooled and filtered off under suction, and the crystalline product was dried in a vacuum drying cabinet.

1. stirringThe mixture was stirred for one hour at room temperature and one hour at 50° C.
2. additionwas then poured over a column
3. additioncontaining 800 ml of strongly basic ion exchanger ("Lewatit" MP 500 OH- -form)
4. washThe exchanger was washed with distilled water
5. customthe runnings collected
6. concentrationwere concentrated to a syrup on a rotary evaporator
7. customThe concentrated syrup was crystallised at 50° C., with addition of a large amount of ethanol
8. additionThe suspension of crystals
9. temperaturewas cooled
10. filtrationfiltered off under suction
11. customthe crystalline product was dried in a vacuum
12. customdrying cabinet

ORDレコード

ord-e937e1966cc341faa74ddbac9b485492

出典データセット

uspto-grants-1986_09

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04611058