Hydrochloric Acid → methyl (S)-3-amino-2-(4-methanesulphonylpiperazin-1-yl)propanoate hydrochloride

HRID 472117노트

반응식

HRID 472117 반응식
[ClH:1].C(OC([NH:9][CH2:10][C@H:11]([N:16]1[CH2:21][CH2:20][N:19]([S:22]([CH3:25])(=[O:24])=[O:23])[CH2:18][CH2:17]1)[C:12]([O:14][CH3:15])=[O:13])=O)(C)(C)C>C(O)(C)C.CO>[ClH:1].[NH2:9][CH2:10][C@H:11]([N:16]1[CH2:21][CH2:20][N:19]([S:22]([CH3:25])(=[O:24])=[O:23])[CH2:18][CH2:17]1)[C:12]([O:14][CH3:15])=[O:13]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 67056930methyl (S)-3-tert-butoxycarbonylamino-2-(4-methanesulfonylpiperazin-1-yl)propanoate

생성물 1

HCID 67057002methyl (S)-3-amino-2-(4-methanesulphonylpiperazin-1-yl)propanoate hydrochloride수율 100%

시약·촉매·용매 2

HCID 887Methanol용매HCID 3776Isopropanol용매

반응 조건

온도
40 °C

실험 절차

15 ml of a solution of hydrochloric acid in isopropanol, having a concentration of 5-6N are added dropwise to a solution of 2.7 g (7.4 mmol) of methyl (S)-3-tert-butoxycarbonylamino-2-(4-methanesulfonylpiperazin-1-yl)propanoate in 30 ml of methanol. The reaction medium is stirred at 40° C. for 2 h, concentrated under vacuum, and then taken up in 20 ml of methanol and 150 ml of diethyl ether. The product precipitates, and is filtered off under vacuum, rinsed with diethyl ether and then dried under vacuum. 2.3 g (100%) of methyl (S)-3-amino-2-(4-methanesulfonylpiperazin-1-yl)propanoate hydrochloride are obtained in the form of a white solid.

후처리

  1. concentrationconcentrated under vacuum
  2. customThe product precipitates
  3. filtrationis filtered off under vacuum
  4. washrinsed with diethyl ether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-714129fb780344edaaa6ebc5363afa7f
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633196B2

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