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

HRID 517496ノート

反応式

HRID 517496 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 3776Isopropanol溶媒

反応条件

温度
40 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-e4356f4eef384808af3d97b6542519d0
出典データセット
uspto-grants-2015_08
特許番号
US09115102B2

反応ノート

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