1,4-Dioxane hydrochloride → 1-{2-[(6-Aminohexanoyl)(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate dihydrochloride

HRID 446511노트

반응식

HRID 446511 반응식
[C:1]1([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8](=[O:35])[O:9][CH:10]1[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][N:18]([C:20](=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH:26]C(OC(C)(C)C)=O)[CH3:19])[CH2:12][CH2:11]1.[ClH:42].O1CCOCC1>O1CCOCC1>[ClH:42].[ClH:42].[C:1]1([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[NH:7][C:8](=[O:35])[O:9][CH:10]1[CH2:11][CH2:12][N:13]([CH2:16][CH2:17][N:18]([C:20](=[O:34])[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][NH2:26])[CH3:19])[CH2:14][CH2:15]1

참가 물질

4

반응물 2

HCID 204431481,4-Dioxane hydrochlorideHCID 666716851-{2-[{6-[(tert-Butoxycarbonyl)amino]hexanoyl}(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate

생성물 1

HCID 666717251-{2-[(6-Aminohexanoyl)(methyl)amino]ethyl}piperidin-4-yl biphenyl-2-ylcarbamate dihydrochloride수율 105.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

The compound (1.59 g, 2.80 mmol) obtained in Example 11b was dissolved in 1,4-dioxane (7 mL), 4 N hydrochloric acid-dioxane (7.00 mL, 28.0 mmol) was added under ice cooling, and the mixture was stirred at room temperature for 20 minutes. Since insoluble material was precipitated, methanol (4 mL) was added, and the mixture was stirred at room temperature for 40 minutes. The solvent was evaporated under reduced pressure to give the title compound (1.60 g; yield, 100%) as a white solid.

후처리

  1. customSince insoluble material was precipitated
  2. additionmethanol (4 mL) was added
  3. stirringthe mixture was stirred at room temperature for 40 minutes
  4. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-9cd9c3d50dab49938357f0c0383896cc
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08476253B2

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