Acetic Acid → 4-Piperazin-1-yl-7-(trifluoromethyl)quinoline

HRID 333984

反応式

HRID 333984 の反応式
Cl[C:2]1[C:11]2[C:6](=[CH:7][C:8]([C:12]([F:15])([F:14])[F:13])=[CH:9][CH:10]=2)[N:5]=[CH:4][CH:3]=1.[NH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.C(O)(=O)C>COCCCOCCCO>[N:16]1([C:2]2[C:11]3[C:6](=[CH:7][C:8]([C:12]([F:15])([F:14])[F:13])=[CH:9][CH:10]=3)[N:5]=[CH:4][CH:3]=2)[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 4837PiperazineHCID 676684-Chloro-7-(trifluoromethyl)quinoline

生成物 1

HCID 114602054-Piperazin-1-yl-7-(trifluoromethyl)quinoline収率 43%

試薬・触媒・溶媒 1

HCID 669843-(3-Methoxypropoxy)-1-propanol溶媒

実験手順

4-Chloro-7-(trifluoromethyl)quinoline (2.3 g, 10 mmol) was dissolved in dipropyleneglycolmonomethyl ether (10 ml) together with piperazine (6.8 g, 0.1 mol) and glacial acetic acid (0.3 ml) and heated at reflux for 2 days. The mixture was concentrated under reduced pressure and the residue was purified by column chromatography (silica, gradient from ethylacetate to methanol containing 1% ammonia) to yield a yellow crystalline solid (1.2 g, 43%).

後処理

  1. temperatureheated
  2. temperatureat reflux for 2 days
  3. concentrationThe mixture was concentrated under reduced pressure
  4. customthe residue was purified by column chromatography (silica, gradient from ethylacetate to methanol containing 1% ammonia)

出典と根拠

ORDレコード
ord-36a1968ea7154fce9d8ee341c05eb17a
出典データセット
uspto-grants-2014_11
特許番号
US08883791B2

関連ノート

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