Potassium Carbonate → 3-Chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile

HRID 885844

反応式

HRID 885844 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8](F)[CH:9]=1)[C:5]#[N:6].[CH3:11][N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([N:15]2[CH2:16][CH2:17][N:12]([CH3:11])[CH2:13][CH2:14]2)[CH:9]=1)[C:5]#[N:6]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 27348413-Chloro-5-fluorobenzonitrile

生成物 1

HCID 591389873-Chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile収率 65.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
140 °C

実験手順

A mixture of 3-chloro-5-fluoro-benzonitrile (1 g, 6.45 mmol), 1-methyl-piperazine (0.715 ml, 6.45 mmol), and K2CO3 (2.64 g, 19.3 mmol) in DMF (5 ml) was heated to 140° C. for 40 min in a microwave apparatus. The resulting slurry was filtered and the solvent was removed in vacuo to give 1 g of 3-chloro-5-(4-methyl-piperazin-1-yl)-benzonitrile. The crude reaction mixture was used in the next step without any further purification.

後処理

  1. filtrationThe resulting slurry was filtered
  2. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-58c40f4ecb7a48bb88aafb20ba0c1bc2
出典データセット
uspto-grants-2012_08
特許番号
US08242175B2

関連ノート

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