HRID63160

反应详情

EQUATION

反应方程式

HRID 63160 的结构方程式

PROCEDURE

实验过程

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 (1,1-dioxidotetrahydro-3-thienyl)amine 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 1.91 (s, 3H), 2.22 (m, 1H), 2.29 (s, 3H), 2.20-2.26 (m, 1H), 2.80-2.91 (m, 1H), 2.95 (bs, 1H), 3.05-3.15 (m, 1H), 3.18-3.24 (m, 1H), 4.69 (bs, 2H), 4.80-4.89 (m, 2H), 5.92 (bs, 1H), 7.17 (t, J=3.9 Hz, 1H), 7.34 (d, J=5.8 Hz, 1H), 7.64 (t, J=6.4 Hz, 1H), 8.57 (d, J=2.8 Hz, 1H); MS (ESI) m/z 348.8 (M+1)+.

WORKUP

后处理

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