Water → HCID 9815399, compound

Temperature

100 °C

A solution of 19.3 mg of trehazolin (prepared as described in Example 1 above) dissolved in 1 ml of 4N aqueous hydrochloric acid was placed in an ampoule and hydrolyzed by heating it at 100° C. for 24 hours. At the end of this time, the reaction mixture was mixed with water and then concentrated to dryness by evaporation under reduced pressure. The residue was again mixed with water and concentrated to dryness by evaporation under reduced pressure, to distill off the hydrochloric acid. The residue from this distillation was dissolved in 20 ml of water, and the pH of the solution was adjusted to a value of 6.0. The resulting solution was passed through a column of 20 ml of Amberlite CG-50 (NH4+)--trade mark--and the column was washed with 60 ml of deionized water and then eluted with 0.2N aqueous ammonia. The eluate was concentrated by evaporation under reduced pressure, and the residue was lyophilized to give 5.1 mg of impure 5-amino-1 -(hydroxymethyl)cyclopentane-1,2,3,4-tetraol as a colorless powder.

1. concentrationconcentrated to dryness by evaporation under reduced pressure
2. additionThe residue was again mixed with water
3. concentrationconcentrated to dryness by evaporation under reduced pressure
4. distillationto distill off the hydrochloric acid
5. distillationThe residue from this distillation
6. dissolutionwas dissolved in 20 ml of water
7. wash(NH4+)--trade mark--and the column was washed with 60 ml of deionized water
8. washeluted with 0.2N aqueous ammonia
9. concentrationThe eluate was concentrated by evaporation under reduced pressure

ORD record

ord-7ec6d68d2dbc46f9bace62532e41685c

Source dataset

uspto-grants-1993_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05260447