Piperidine → Benzoic acid, 3-nitro-4-(1-piperidinyl)-, methyl ester

HRID 406391ノート

反応式

HRID 406391 の反応式
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.F[C:8]1[CH:17]=[CH:16][C:11]([C:12]([O:14][CH3:15])=[O:13])=[CH:10][C:9]=1[N+:18]([O-:20])=[O:19]>CN(C=O)C.C(OCC)(=O)C>[N+:18]([C:9]1[CH:10]=[C:11]([CH:16]=[CH:17][C:8]=1[N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1)[C:12]([O:14][CH3:15])=[O:13])([O-:20])=[O:19]

参加物

5

反応物 2

HCID 8082PiperidineHCID 5219721Methyl 4-fluoro-3-nitrobenzoate

生成物 1

HCID 2878938Benzoic acid, 3-nitro-4-(1-piperidinyl)-, methyl ester

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Piperidine (1.24 ml) was added to a solution of methyl 4-fluoro-3-nitrobenzoate (1.00 g) in DMF (20 ml) and the mixture was stirred at room temperature for 1 hour. The reaction mixture was diluted with ethyl acetate, sequentially washed with water and brine, and dried over anhydrous sodium sulfate. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to obtain the title compound (1.50 g).

後処理

  1. washsequentially washed with water and brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-f75e44dcf4314daaae7c41e3b371dbdc
出典データセット
uspto-grants-2014_06
特許番号
US08754100B2

反応ノート

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