2-Chloro-4-cyanopyridine → 2-(4-Cyclopentyl-piperazin-1-yl)-isonicotinonitrile

HRID 272531ノート

反応式

HRID 272531 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]#[N:9])[CH:5]=[CH:4][N:3]=1.[CH:10]1([N:15]2[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]2)[CH2:14][CH2:13][CH2:12][CH2:11]1>CN(C=O)C>[CH:10]1([N:15]2[CH2:16][CH2:17][N:18]([C:2]3[CH:7]=[C:6]([CH:5]=[CH:4][N:3]=3)[C:8]#[N:9])[CH2:19][CH2:20]2)[CH2:11][CH2:12][CH2:13][CH2:14]1

参加物

4

反応物 2

HCID 5686382-Chloro-4-cyanopyridineHCID 8064211-Cyclopentylpiperazine

生成物 1

HCID 623696172-(4-Cyclopentyl-piperazin-1-yl)-isonicotinonitrile収率 94.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A mixture of 2 g (14 mmol) 2-chloro-4-cyanopyridine and 2.34 g (15 mmol) 1-cyclopentylpiperazine in 5 ml DMF was heated to 80° C. for 16 h. The mixture was evaporated under reduced pressure and the residue was treated with 100 ml 1M NaHCO3 aq. and extracted with two times 100 ml ethyl acetate. The combined organic phases were dried with MgSO4 and evaporated under reduced pressure to yield 3.4 g (92%) of the title compound as grey solid. (m/e): 257.3 (MH+; 100%).

後処理

  1. customThe mixture was evaporated under reduced pressure
  2. additionthe residue was treated with 100 ml 1M NaHCO3 aq.
  3. extractionextracted with two times 100 ml ethyl acetate
  4. dry with materialThe combined organic phases were dried with MgSO4
  5. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-65ddd3cf0d6f424d92d5d5ed38221ab5
出典データセット
uspto-grants-2008_11
特許番号
US07456175B2

反応ノート

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