HCID 59204985、化合物 → 1-(2-Fluoro-4-nitrophenyl)piperidine-4-ylmethylamine

HRID 2241904ノート

反応式

HRID 2241904 の反応式
C(=[N:8][CH2:9][CH:10]1[CH2:15][CH2:14][N:13]([C:16]2[CH:21]=[CH:20][C:19]([N+:22]([O-:24])=[O:23])=[CH:18][C:17]=2[F:25])[CH2:12][CH2:11]1)C1C=CC=CC=1>Cl>[F:25][C:17]1[CH:18]=[C:19]([N+:22]([O-:24])=[O:23])[CH:20]=[CH:21][C:16]=1[N:13]1[CH2:12][CH2:11][CH:10]([CH2:9][NH2:8])[CH2:15][CH2:14]1

参加物

3

反応物 1

HCID 59204985HCID 59204985、化合物

生成物 1

HCID 592050221-(2-Fluoro-4-nitrophenyl)piperidine-4-ylmethylamine収率 98.5%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

1N aqueous hydrochloric acid (20 ml) was added to benzylidene[1-(2-fluoro-4-nitrophenyl)piperidine-4-ylmethyl]amine (compound of Reference Example 21; 1.15 g, 3.36 mmol), and the mixture was refluxed for 6 hours. The reaction mixture was washed with ethyl acetate and adjusted to pH=12 by addition of 2N aqueous sodium hydroxide. The water layer was saturated with sodium chloride and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to give the title compound (0.838 g, 98%) as a yellow solid.

後処理

  1. temperaturethe mixture was refluxed for 6 hours
  2. washThe reaction mixture was washed with ethyl acetate
  3. additionadjusted to pH=12 by addition of 2N aqueous sodium hydroxide
  4. extractionextracted with chloroform
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customThe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-05a0af01464f43a8a51e86e304bd3a47
出典データセット
uspto-grants-2010_03
特許番号
US07671058B2

反応ノート

読み込み中…