反応 #91435

反応方程式

N4-cyclopentyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine

o-toluidine

→

titled compound

5,6-dimethyl-N4-(2-methylphenyl)-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine

反応条件

後処理

1. 1
   その他The titled compound was synthesized
2. 2
   その他The crude material was purified by column chromatography
3. 3
   洗浄eluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1)
4. 4
   洗浄the final product was washed with diethyl ether

実験手順

The titled compound was synthesized according to the procedure described for preparation of N4-cyclopentyl-5,6-dimethyl-N2-(pyridin-2-ylmethyl)pyrimidine-2,4-diamine (Example 29) using o-toluidine instead of cyclopentanamine. The crude material was purified by column chromatography eluting with mixture of chloroform/ethanol/20% water solution of ammonia (200:10:1), and then the final product was washed with diethyl ether to afford the titled compound as a white solid. 1H NMR (300 MHz, CDCl3) δ ppm 2.08 (s, 3H), 2.27 (s, 3H), 2.34 (s, 3H), 4.66 (d, J=3.2 Hz, 2H), 5.70 (bs, 1H), 6.14 (s, 1H), 7.01 (t, J=6.3 Hz, 1H), 7.13 (t, J=6.3 Hz, 2H), 7.18 (d, J=7.5 Hz, 1H), 7.24 (d, J=7.8 Hz, 1H), 7.58 (t, J=7.8 Hz, 1H), 7.84 (d, J=7.8 Hz, 1H), 8.54 (d, J=4.8 Hz, 1H); MS (ESI) m/z 320.7 (M+1)+.

出典