Hydrochloric Acid → (2S)-2-Methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine hydrochloride

HRID 418276ノート

反応式

HRID 418276 の反応式
[CH3:1][C@@H:2]1[N:7]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH2:6][CH2:5][N:4](C(OC(C)(C)C)=O)[CH2:3]1.[ClH:28]>O1CCOCC1>[ClH:28].[CH3:1][C@H:2]1[CH2:3][NH:4][CH2:5][CH2:6][N:7]1[S:8]([C:11]1[CH:12]=[CH:13][C:14]([C:17]([F:20])([F:18])[F:19])=[CH:15][CH:16]=1)(=[O:10])=[O:9]

参加物

4

反応物 2

HCID 313Hydrochloric Acid2 回HCID 591521131,1-dimethylethyl(3S)-3-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinecarboxylate

生成物 1

HCID 66649356(2S)-2-Methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine hydrochloride収率 102.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a solution of 1,1-dimethylethyl(3S)-3-methyl-4-{[4-(trifluoromethyl)phenyl]sulfonyl}-1-piperazinecarboxylate (may be prepared as described in Description 5) (4.40 g, 10.8 mmol) in 1,4-dioxane (30 ml) was added HCl (4M in 1,4-dioxane) (5.39 ml, 21.6 mmol) and the mixture stirred at rt for 2 hours. A further portion of HCl (4M in 1,4-dioxane) (16.2 ml, 64.6 mmol) was then added and the mixture stirred for a further 16 hours. The volatiles were then removed in vacuo to give the title compound (3.80 g) as a white solid.

後処理

  1. stirringthe mixture stirred for a further 16 hours
  2. customThe volatiles were then removed in vacuo

出典と根拠

ORDレコード
ord-25377cb524854f32b668279485bc9f01
出典データセット
uspto-grants-2012_01
特許番号
US08093249B2

反応ノート

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