Hydrochloric Acid → 1-(4-Nitrobenzenesulfonyl)piperidin-4-amine

HRID 337199노트

반응식

HRID 337199 반응식
C(OC(=O)[NH:7][CH:8]1[CH2:13][CH2:12][N:11]([S:14]([C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-:25])=[O:24])=[CH:19][CH:18]=2)(=[O:16])=[O:15])[CH2:10][CH2:9]1)(C)(C)C.Cl>O1CCOCC1>[N+:23]([C:20]1[CH:19]=[CH:18][C:17]([S:14]([N:11]2[CH2:10][CH2:9][CH:8]([NH2:7])[CH2:13][CH2:12]2)(=[O:15])=[O:16])=[CH:22][CH:21]=1)([O-:25])=[O:24]

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 71079538[1-(4-Nitro-benzenesulfonyl)-piperidin-4-yl]carbamic acid tert-butyl ester

생성물 1

HCID 284183251-(4-Nitrobenzenesulfonyl)piperidin-4-amine수율 89.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

[1-(4-Nitro-benzenesulfonyl)-piperidin-4-yl]-carbamic acid tert-butyl ester (3.5 g, 9.0 mmol) was suspended in a 4M solution of HCl in Dioxane (100 ml). The resulting suspension was stirred at room temperature for 3 hours. After this time the solution was concentrated under vacuum, then azeotroped with methanol and suspended in diethyl ether. The resulting solid precipitate was then collected by filtration, washed with diethyl ether and dried under vacuum to afford the title compound (2.3 g, 86% yield) as a white solid. Tr=1.10 min, m/z (ES+) (M+H)+ 286.

후처리

  1. concentrationAfter this time the solution was concentrated under vacuum
  2. customazeotroped with methanol
  3. filtrationThe resulting solid precipitate was then collected by filtration
  4. washwashed with diethyl ether
  5. customdried under vacuum

출처 및 근거

ORD 기록
ord-9ddad51d7ab041b893c69633222a2db4
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08889716B2

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