반응 #91429

ord-ddb85890747f46fb8ea927465102b1f5

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

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

실험 절차

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 1,3-benzodioxol-5-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 2.04 (s, 3H), 2.32 (s, 3H), 4.69 (d, J=4.2 Hz, 2H), 5.76 (bs, 1H), 5.95 (s, 2H), 6.22 (s, 1H), 6.67-7.75 (m, 2H), 7.14 (t, J=6.4 Hz, 1H), 7.21 (s, 1H), 7.32 (d, J=7.8 Hz, 1H), 7.60 (t, J=7.6 Hz, 1H), 8.56 (d, J=3.6 Hz, 1H); MS (ESI) m/z 350.7 (M+1)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09447051B2uspto-grants-2016_09