Hydrochloric Acid → 1-(trans-4-Glycylamino-L-prolyl)-4-(3,5-dichlorophenoxy)piperidine Dihydrochloride

HRID 2185482노트

반응식

HRID 2185482 반응식
[ClH:1].C(OC([NH:9][CH2:10][C:11]([NH:13][C@H:14]1[CH2:18][N:17](C(OC(C)(C)C)=O)[C@H:16]([C:26]([N:28]2[CH2:33][CH2:32][CH:31]([O:34][C:35]3[CH:40]=[C:39]([Cl:41])[CH:38]=[C:37]([Cl:42])[CH:36]=3)[CH2:30][CH2:29]2)=[O:27])[CH2:15]1)=[O:12])=O)(C)(C)C>O1CCOCC1>[ClH:41].[ClH:1].[NH2:9][CH2:10][C:11]([NH:13][C@H:14]1[CH2:18][NH:17][C@H:16]([C:26]([N:28]2[CH2:33][CH2:32][CH:31]([O:34][C:35]3[CH:36]=[C:37]([Cl:42])[CH:38]=[C:39]([Cl:41])[CH:40]=3)[CH2:30][CH2:29]2)=[O:27])[CH2:15]1)=[O:12]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 701730401-[trans-4-(n-Tert-butoxycarbonylglycylamino)-n-tert-butoxycarbonyl-l-prolyl]-4-(3,5-dichlorophenoxy)piperidine

생성물 1

HCID 701757581-(trans-4-Glycylamino-L-prolyl)-4-(3,5-dichlorophenoxy)piperidine Dihydrochloride

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

A solution of 4 N hydrochloric acid in 1,4-dioxane (13 mL) was added to a solution of 1-[trans-4-(N-tert-butoxycarbonylglycylamino)-N-tert-butoxycarbonyl-L-prolyl]-4-(3,5-dichlorophenoxy)piperidine (C, 640 mg) in 1,4-dioxane (13 mL) at room temperature. After stirring at room temperature for 30 min, the reaction mixture was evaporated in vacuo. The residue was washed with ether to give the titled compound (361 mg) as white crystals: 1H NMR (400 MHz, D2O) δ 1.80 (br s, 2H), 2.03 (br s, 2H), 2.40 (m, 1H), 2.61 (m, 1H), 3.46-3.50 (m, 2H), 3.60 (br s, 1H), 3.77 (m, 3H), 3.86 (s, 2H), 4.58 (br s, 1H), 4.72 (br s, 1H), 5.03 (t, J=8.3 Hz, 1H), 7.03 (br s, 2H), and 7.10 (br s, 1H); mass spectrum (EI+) m/e 415.

후처리

  1. customthe reaction mixture was evaporated in vacuo
  2. washThe residue was washed with ether

출처 및 근거

ORD 기록
ord-53b79b06cd154c7d823bf7859295fbc3
출처 데이터셋
uspto-grants-2002_06
특허 번호
US06399629B1

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