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Hydrochloric Acid → 6-Amino-N-(pyridin-3-yl)hexanoamide Dihydrochloride

HRID 1255100
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반응식

HRID 1255100 반응식
C(OC(=O)[NH:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13](=[O:21])[NH:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)(C)(C)C.[ClH:23]>C(Cl)Cl.O1CCOCC1>[ClH:23].[ClH:23].[NH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][C:13]([NH:14][C:15]1[CH:16]=[N:17][CH:18]=[CH:19][CH:20]=1)=[O:21]
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 66810297(5-(Pyridin-3-ylcarbamoyl)pentyl]carbamic acid tert-butyl ester

생성물 1

HCID 668104466-Amino-N-(pyridin-3-yl)hexanoamide Dihydrochloride

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 312751,4-Dioxane용매

실험 절차

To an ice-cold mixture of (5-(Pyridin-3-ylcarbamoyl)pentyl)carbamic acid tert-butyl ester (3, 3.07 g, 10 mmole) in methylene chloride (30 mL) was added a solution of HCl in dioxane (4M, 10 mL). The mixture was stirred at room temperature overnight. The separated solid was filtered, washed with methylene chloride, dried in vacuum oven to give the product 4 as the hydrochloride salt (2.7 g, 96%). The 1H NMR spectrum of the pure solid was consistent with structure 4. 1H NMR (D2O) δ 9.20 (s, 2H), 7.91 (m, 1H), 2.90 (t, 2H), 2.42 (t, 2H), 2.62 (m, 4H), 1.36 (m, 2H).

후처리

  1. filtrationThe separated solid was filtered
  2. washwashed with methylene chloride
  3. customdried in vacuum oven

출처 및 근거

ORD 기록
ord-4a383a7a40f34099a885cf5cff819055
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08455688B2

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