Hydrochloric Acid → 1-(trans-4-Aminomethyl-L-Prolyl)-4-(3-Chloro-2-Methylphenyl)piperazine Dihydrochloride

HRID 2185470ノート

反応式

HRID 2185470 の反応式
[ClH:1].C(OC([NH:9][CH2:10][C@H:11]1[CH2:15][N:14](C(OC(C)(C)C)=O)[C@H:13]([C:23]([N:25]2[CH2:30][CH2:29][N:28]([C:31]3[CH:36]=[CH:35][CH:34]=[C:33]([Cl:37])[C:32]=3[CH3:38])[CH2:27][CH2:26]2)=[O:24])[CH2:12]1)=O)(C)(C)C>O1CCOCC1>[ClH:37].[ClH:1].[NH2:9][CH2:10][C@H:11]1[CH2:15][NH:14][C@H:13]([C:23]([N:25]2[CH2:30][CH2:29][N:28]([C:31]3[CH:36]=[CH:35][CH:34]=[C:33]([Cl:37])[C:32]=3[CH3:38])[CH2:27][CH2:26]2)=[O:24])[CH2:12]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 540742211-[trans-4-(n-Tert-butoxycarbonylaminomethyl)-n-tert-butoxycarbonyl-l-prolyl]-4-(3-chloro-2-methylphenyl)piperazine

生成物 1

HCID 701753811-(trans-4-Aminomethyl-L-Prolyl)-4-(3-Chloro-2-Methylphenyl)piperazine Dihydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of 4 N hydrochloric acid in 1,4-dioxane (3 mL) was added to a solution of 1-[trans-4-(N-tert-butoxycarbonylaminomethyl)-N-tert-butoxycarbonyl-L-prolyl]-4-(3-chloro-2-methylphenyl)piperazine (B, 98 mg) in 1,4-dioxane (3 mL) at room temperature. After stirring at room temperature for 20 min, the reaction mixture was concentrated in vacuo. The residue was washed with ether to give the titled compound (61 mg) as a white powder: 1H NMR (400 MHz, ) δ 2.37 (s, 3H), 2.40-2.47 (br s, 2H), 2.83 (br s, 1H), 3.07 (br s, 4H), 3.32 (br s, 3H), 3.77 (m, 5H), 5.02 (br s, 1H), 7.09 (m, 1H), and 7.25 (m, 2H).

後処理

  1. concentrationthe reaction mixture was concentrated in vacuo
  2. washThe residue was washed with ether

出典と根拠

ORDレコード
ord-6aedb950e120433ea5b5b9d0cb3e263c
出典データセット
uspto-grants-2002_06
特許番号
US06399629B1

反応ノート

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