反応 #60019

反応方程式

2-(2-Aminoethylamino)pyridine

2-chloropyridine

ethylenediamine

Ether

benzotriazole carboxamidinium

DIEA

→

title compound

4-(2-{[2-(2-pyridylamino)ethyl]amino}pyrimidin-4-yl)benzamide

溶媒

acetonitrile

反応条件

後処理

1. 1
   ろ過After 8 hours the white solid amino[2-(2-pyridylamino)ethyl]carboxamidinium 4-methylbenzenesulfonate was filtered off
2. 2
   その他dried in vacuo
3. 3
   その他The resulting guanidine (200 mg) was reacted with 100 mg of resin (21 hours, 90° C.)

実験手順

2-(2-Aminoethylamino)pyridine (prepared from 2-chloropyridine and ethylenediamine in accordance with the method described in T. Mega et al., 1988, Bull. Chem. Soc. Japan 61:4315, which is incorporated herein by reference) (6 mmol) was treated with benzotriazole carboxamidinium 4-methylbenzenesulfonatesulfonate (2.0 g, 6 mmol) and DIEA (1.05 ml, 6 mmol) in anhydrous acetonitrile (10 ml) for 65 hours. Ether (ca. 10 ml) was then added to this mixture. After 8 hours the white solid amino[2-(2-pyridylamino)ethyl]carboxamidinium 4-methylbenzenesulfonate was filtered off and dried in vacuo. The resulting guanidine (200 mg) was reacted with 100 mg of resin (21 hours, 90° C.) according to the method described in Example 10 (Resin method C), to give the title compound.

出典