Hydrochloric Acid → L-Aspartic acid diethyl ester hydrochloride

HRID 993476노트

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HRID 993476 반응식
[C:1]([Cl:4])(=O)[CH3:2].Cl.[NH2:6][C@H:7]([C:12]([OH:14])=[O:13])[CH2:8][C:9]([OH:11])=[O:10].[CH2:15](O)[CH3:16]>>[ClH:4].[NH2:6][C@H:7]([C:12]([O:14][CH2:1][CH3:2])=[O:13])[CH2:8][C:9]([O:11][CH2:15][CH3:16])=[O:10]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 5960L-Aspartic AcidHCID 6367Acetyl chloride

생성물 1

HCID 12416466L-Aspartic acid diethyl ester hydrochloride

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온도
25 °C

실험 절차

Absolute ethanol (420 ml) was cooled in ice and acetyl chloride (71.4 ml, 1.03 mol) was added dropwise to generate HCl in situ. After the addition, the reaction was stirred for additional 30 minutes. L-Aspartic acid (33.27 g, 0.25 mol) was added in one portion and the solution heated slowly after dissolution to reflux. Refluxing was continued until the reaction was complete (TLC). The reaction mixture was then cooled to 25° C. and the solvent was removed under reduced pressure. Further drying under vacuum gave crude diethyl L-aspartate hydrochloride 2 as a viscous oil which crystallised on standing to a white solid, yield: 60 g (100%). This material was used without further purification. Spectral data for this sample were consistent with those given in the literature1. 13C NMR (75 MHz, d6-DMSO) 169.1, 168.2, 70.0, 60.9, 48.5, 34.2, 14.9 and 13.9.

후처리

  1. additionAfter the addition
  2. temperaturethe solution heated slowly
  3. dissolutionafter dissolution
  4. temperatureto reflux
  5. temperatureRefluxing
  6. customthe solvent was removed under reduced pressure
  7. customFurther drying under vacuum

출처 및 근거

ORD 기록
ord-a56a4f74157f44afb6d28328400b8104
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06472533B1

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