Tert-butyl 4-(4-chlorophenylamino)piperidine-1-carboxylate → N-(4-chlorophenyl)piperidin-4-amine

HRID 856073ノート

反応式

HRID 856073 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH:9]2[CH2:14][CH2:13][N:12](C(OC(C)(C)C)=O)[CH2:11][CH2:10]2)=[CH:4][CH:3]=1>C(Cl)Cl.FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 1491503Tert-butyl 4-(4-chlorophenylamino)piperidine-1-carboxylate

生成物 1

HCID 7183033N-(4-chlorophenyl)piperidin-4-amine

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

Tert-butyl 4-(4-chlorophenylamino)piperidine-1-carboxylate (2.67 g, 8.59 mmol) prepared in Reference Example 131 was dissolved in methylene chloride (20 ml), to which trifluoroacetic acid (15 ml) was added dropwise, and the mixture was stirred at room temperature for 5 hours. The reaction mixture was concentrated under reduced pressure, and the residue was then dissolved in methylene chloride. This solution was neutralized with sodium hydroxide aqueous solution, and the mixture was extracted with methylene chloride. The extract was washed with brine, dried over magnesium sulfate, and then filtered. The filtrate was concentrated under reduced pressure to afford 4-(4-chlorophenylamino)piperidine as a pale yellow powder.

後処理

  1. additionwas added dropwise
  2. concentrationThe reaction mixture was concentrated under reduced pressure
  3. dissolutionthe residue was then dissolved in methylene chloride
  4. extractionthe mixture was extracted with methylene chloride
  5. washThe extract was washed with brine
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-b7e0b26ef41843808d9e512db4e5bd34
出典データセット
uspto-grants-2007_08
特許番号
US07262212B2

反応ノート

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