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

HRID 2185470노트

반응식

HRID 2185470 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

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).

후처리

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

출처 및 근거

ORD 기록
ord-6aedb950e120433ea5b5b9d0cb3e263c
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399629B1

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