Hydrochloric Acid → N,N-dimethyl-1-(4-nitrophenyl)piperidin-4-amine

HRID 1348563

反応式

HRID 1348563 の反応式
Cl.Cl.[CH3:3][N:4]([CH3:11])[CH:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1.F[C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=1.Cl>CO>[CH3:3][N:4]([CH3:11])[CH:5]1[CH2:10][CH2:9][N:8]([C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=2)[CH2:7][CH2:6]1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 9590p-FluoronitrobenzeneHCID 225914404-(Dimethylamino)piperidine dihydrochloride

生成物 1

HCID 11086151N,N-dimethyl-1-(4-nitrophenyl)piperidin-4-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

反応条件

温度
90 °C

実験手順

Dimethyl-piperidin-4-yl-amine dihydrochloride (Aldrich, 2.0 g, 9.95 mmol) and 4-fluoro-nitrobenzene (Aldrich, 2.5 g, 17.7 mmol) were added to methanol (30 mL). The mixture was heated to 90° C. and stirred for 3.5 hours. The mixture was treated with 1 N HCl to pH=1 and then extracted with diethyl ether (2×10 mL). The aqueous layer was treated with saturated sodium carbonate to pH=10 and then extracted with methylene chloride (2×20 mL). The organic layer was dried with sodium sulfate and the solvent was removed to give the desired product. 1.25 g, 50%. MS (m+H)+: 250.

後処理

  1. extractionextracted with diethyl ether (2×10 mL)
  2. additionThe aqueous layer was treated with saturated sodium carbonate to pH=10
  3. extractionextracted with methylene chloride (2×20 mL)
  4. dry with materialThe organic layer was dried with sodium sulfate
  5. customthe solvent was removed

出典と根拠

ORDレコード
ord-7a4df0aa5ce14d80a59cf2829f16ebe3
出典データセット
uspto-grants-2007_05
特許番号
US07211576B2

関連ノート

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