Trifluoroacetic acid → 1-(6-Chloro-pyridin-3-yl)-homopiperazine

HRID 2416608

反応式

HRID 2416608 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([N:8]2[CH2:14][CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 224784871-(6-Chloro-3-pyridyl)-4-tert-butoxycarbonyl homopiperazine

生成物 1

HCID 98343281-(6-Chloro-pyridin-3-yl)-homopiperazine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 1-(6-chloro-3-pyridyl)-4-tert-butoxycarbonyl homopiperazine (1.7 g, 5.5 mmol), trifluoro acetic acid (4.5 ml, 55 mmol) and dichloromethane at room temperature for 1 h. The mixture was evaporated. Chromatography on silica gel with a mixture of petroleum:ethyl acetate (1:1) gave the title compound as free base. The corresponding salt was obtained by addition of a diethyl ether and methanol mixture (9:1) saturated with fumaric acid. Mp 165-167° C. Yield 0.72 g, 40%.

後処理

  1. customThe mixture was evaporated
  2. additionChromatography on silica gel with a mixture of petroleum:ethyl acetate (1:1)

出典と根拠

ORDレコード
ord-b5bfe982ec264d5e8bf894f0248c97e4
出典データセット
uspto-grants-2004_11
特許番号
US06825189B1

関連ノート

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