Alanine methyl ester hydrochloride → HCID 87830865, compound

L-Ala-OMe HCl salt (1.00 g, 7.16 mmol) was suspended in methyl acetate (15 ml), and benzenesulfonic acid monohydrate (BsOH H2O) (1.51 g, 8.57 mmol) was added. The mixture was stirred for dissolution. This solution was concentrated under reduced pressure, and methyl acetate (15 ml) was added. The mixture was concentrated twice under reduced pressure, and the obtained concentrate was cooled in a refrigerator. Since partial crystallization occurred, diethyl ether (3 ml) and methyl acetate (15 ml) were added to dissolve the crystals almost entirely at 40° C. This solution was stirred at room temperature and cooled overnight in a refrigerator. The crystals were separated and dried to give L-alanine methyl ester benzenesulfonate (L-Ala-OMe BsOH salt) crystals. The crystals were left standing at room temperature for a while. As a result, the crystals were liquefied and failed to provide stable crystals.

1. concentrationThis solution was concentrated under reduced pressure, and methyl acetate (15 ml)
2. additionwas added
3. concentrationThe mixture was concentrated twice under reduced pressure
4. concentrationthe obtained concentrate
5. temperaturewas cooled in a refrigerator
6. customSince partial crystallization
7. additiondiethyl ether (3 ml) and methyl acetate (15 ml) were added
8. dissolutionto dissolve the crystals almost entirely at 40° C
9. stirringThis solution was stirred at room temperature
10. temperaturecooled overnight in a refrigerator
11. customThe crystals were separated
12. customdried

ORD record

ord-a6c4c991277f457bb6108fd023fea4c5

Source dataset

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07205433B2