반응 #91406

ord-eade01c632694bf195c4a9387c8ce857

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 3,4-dihydro-2H-chromen-4-ylamine 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 (400 MHz, CDCl3) δ ppm 1.89 (s, 3H), 2.10 (bs, 1H), 2.42 (s, 3H), 4.11 (bs, 1H), 4.27 (bs, 1H), 4.93 (bs, 1H), 5.04 (bs, 1H), 5.31 (bs, 1H), 5.48 (bs, 1H), 6.75-6.88 (m, 3H), 7.20 (bs, 1H), 7.27 (bs, 1H), 7.42 (bs, 1H), 7.74 (bs, 1H), 8.02 (bs, 1H), 8.59 (bs, 1H), 10.63 (bs, 1H); MS (ESI) m/z 362.9 (M+1)+.

출처

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