4-Ethylbenzenesulfonic acid → L-alanine methyl ester 4-ethylbenzenesulfonate

L-Ala-OMe HCl salt (1.00 g, 7.16 mmol) was suspended in methyl acetate (15 ml). 4-Ethylbenzenesulfonic acid (4-EBS) (1.60 g, 8.57 mmol) was added, and the mixture was stirred for dissolution. This solution was concentrated under reduced pressure, methyl acetate (15 ml) was added, and the mixture was concentrated twice under reduced pressure. The obtained concentrate was cooled in a refrigerator. Since partial crystallization occurred, methyl acetate (15 ml) was added to dissolve the crystals at 50° C. This solution was stirred at room temperature to give a slurry. This slurry was cooled overnight in a refrigerator and the crystals were separated and dried to give 1.04 g of L-alanine methyl ester 4-ethylbenzenesulfonate (L-Ala-OMe 4-EBS salt) dry crystals (L-Ala-OMe 4-EBS salt content 100%, 3.42 mmol, yield 47.8%).

1. concentrationThis solution was concentrated under reduced pressure, 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. additionmethyl acetate (15 ml) was added
8. dissolutionto dissolve the crystals at 50° C
9. stirringThis solution was stirred at room temperature
10. customto give a slurry
11. temperatureThis slurry was cooled overnight in a refrigerator
12. customthe crystals were separated
13. customdried

ORDレコード

ord-37cb5e62cf7a42c4bf23e2e439db5a18

出典データセット

uspto-grants-2007_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07205433B2