Hydrochloric Acid → HCID 67908176, compound

Temperature

60 °C

A mixture of 1 g of the product of Example 2, 8 ml of demineralized water and 0.8 ml of hydrochloric acid was sitrred at 20° C. for one hour and was then heated at 60° C. for one hour and was cooled at 20° C. The mixture was diluted with 15 ml of water and was then extracted with methylene chloride. The organic phase was washed with aqueous N sodium hydroxide solution and with water until the wash water was neutral, dried and evaporated to dryness under reduced pressure. The residue was taken up in 10 ml of ether and a stream of hydrogen chloride was slowly bubbled therethrough. The mixture was vacuum filtered to obtain 350 mg of benzyl L-leucine hydrochloride melting at 135° C. and having a specific rotation of [α]D20 =-5.5°±1° (c=1% in 0.1N hydrochloric acid).

1. temperaturewas cooled at 20° C
2. extractionwas then extracted with methylene chloride
3. washThe organic phase was washed with aqueous N sodium hydroxide solution and with water until the wash water
4. customdried
5. customevaporated to dryness under reduced pressure
6. customa stream of hydrogen chloride was slowly bubbled
7. filtrationfiltered

ORD record

ord-1bf3a51eb8a047e1acb6b5e8c717d143

Source dataset

uspto-grants-1992_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05136050