Trifluoroacetic acid → 1-{1-[4-(Trifluoromethyl)phenyl]piperidin-4-yl}methanamine

HRID 2093586ノート

反応式

HRID 2093586 の反応式
FC(F)(F)C(O)=O.C(OC(=O)[NH:14][CH2:15][CH:16]1[CH2:21][CH2:20][N:19]([C:22]2[CH:27]=[CH:26][C:25]([C:28]([F:31])([F:30])[F:29])=[CH:24][CH:23]=2)[CH2:18][CH2:17]1)(C)(C)C>ClCCl>[F:30][C:28]([F:29])([F:31])[C:25]1[CH:24]=[CH:23][C:22]([N:19]2[CH2:20][CH2:21][CH:16]([CH2:15][NH2:14])[CH2:17][CH2:18]2)=[CH:27][CH:26]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 66853254Tert-butyl({1-[4-(trifluoromethyl)phenyl]piperidin-4-yl}methyl)carbamate

生成物 1

HCID 595860101-{1-[4-(Trifluoromethyl)phenyl]piperidin-4-yl}methanamine収率 123.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of trifluoroacetic acid (10 ml) and dichloromethane (10 ml) was added to tert-butyl({1-[4-(trifluoromethyl)phenyl]piperidin-4-yl}methyl)carbamate (1.36 g). This mixture was stirred at room temperature for 3 h. The sample was concentrated and taken up in dichloromethane (20 ml) and saturated aqueous sodium bicarbonate. The mixture was extracted and the organic layer was dried over sodium sulfate, filtered, and concentrated in vacuo to provide the title compound (1.21 g, 86%). Mass spectrum (ESI) 242.1 (M+1).

後処理

  1. concentrationThe sample was concentrated
  2. extractionThe mixture was extracted
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-071f88bfa2834bc49a00051e172efd00
出典データセット
uspto-grants-2013_05
特許番号
US08445480B2

反応ノート

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