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

HRID 337199ノート

反応式

HRID 337199 の反応式
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]

参加物

4

反応物 2

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

生成物 1

HCID 284183251-(4-Nitrobenzenesulfonyl)piperidin-4-amine収率 89.6%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

[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.

後処理

  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

出典と根拠

ORDレコード
ord-9ddad51d7ab041b893c69633222a2db4
出典データセット
uspto-grants-2014_11
特許番号
US08889716B2

反応ノート

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