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

HRID 517496노트

반응식

HRID 517496 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-methanesulphonylpiperazin-1-yl)propanoate in 30 ml of methanol. The reaction medium is stirred at 40° C. for 2 h, concentrated under vacuum then taken up in 20 ml of methanol and 150 ml of diethyl ether. The product precipitates, is filtered, rinsed with diethyl ether then dried under vacuum. 2.3 g (100%) of methyl (S)-3-amino-2-(4-methanesulphonylpiperazin-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
  4. washrinsed with diethyl ether
  5. customthen dried under vacuum

출처 및 근거

ORD 기록
ord-e4356f4eef384808af3d97b6542519d0
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09115102B2

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