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

HRID 1271656

반응식

HRID 1271656 반응식
[NH2:1][C@H:2]([C:4]([O:6][CH3:7])=[O:5])[CH3:3].Cl.[CH2:9]([C:11]1[CH:16]=[CH:15][C:14]([S:17]([OH:20])(=[O:19])=[O:18])=[CH:13][CH:12]=1)[CH3:10]>C(OC)(=O)C>[CH2:9]([C:11]1[CH:12]=[CH:13][C:14]([S:17]([OH:20])(=[O:18])=[O:19])=[CH:15][CH:16]=1)[CH3:10].[CH3:7][O:6][C:4](=[O:5])[C@H:2]([CH3:3])[NH2:1]

참가 물질

4

반응물 2

HCID 74024-Ethylbenzenesulfonic acidHCID 2733257Alanine methyl ester hydrochloride

생성물 1

HCID 10334362L-alanine methyl ester 4-ethylbenzenesulfonate수율 50.2%

시약·촉매·용매 1

HCID 6584Methyl Acetate용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-37cb5e62cf7a42c4bf23e2e439db5a18
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07205433B2

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