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

HRID 517501
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반응식

HRID 517501 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]
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 67056910methyl (R)-3-tert-butoxycarbonylamino-2-(4-methanesulphonyl-piperazin-1-yl)propanoate

생성물 1

HCID 67056954methyl (R)-3-amino-2-(4-methanesulphonylpiperazin-1-yl)propanoate hydrochloride수율 97%

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 3.8 g (10.4 mmol) of methyl (R)-3-tert-butoxycarbonylamino-2-(4-methanesulphonylpiperazin-1-yl)propanoate in 50 ml of methanol. The reaction medium is stirred at 40° C. for 3 h, concentrated under vacuum then taken up in diethyl ether. The product precipitates, is filtered, rinsed with diethyl ether then dried under vacuum. 3 g (97%) of methyl (R)-3-amino-2-(4-methanesulphonylpiperazin-1-yl)propanoate hydrochloride are obtained in the form of a beige solid.

후처리

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

출처 및 근거

ORD 기록
ord-a30cd320a53749c29211a019bf456ace
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115102B2

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