반응 #2353271

ord-12cfe47e6e7245faa892decdfd47685e

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타formed
  2. 2
    기타The solid that had formed
  3. 3
    여과was collected by filtration
  4. 4
    세척washed with diethyl ether
  5. 5
    기타dried under vacuum at 45 C
  6. 6
    기타to give 171 mg

실험 절차

5-(6-Isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-pyrimidine-2,4-diamine was prepared from 2-(6-isopropyl-1,3-dimethyl-1H-indol-5-yloxy)-4-methoxy-but-2-enenitrile by treatment with guanidine carbonate and sodium methoxide using the procedure of step 7 of Example 2 above. This material was dissolved in 2.5 ml absolute ethanol, and 820 ml of 1 N HCl in diethyl ether was added with stirring. Diethyl ether was added slowly until small crystals formed, and the solution was then placed in a −10 C freezer for 18 hours. The solid that had formed was collected by filtration, washed with diethyl ether, and dried under vacuum at 45 C to give 171 mg. of the hydrochloride salt, Mp: 185.1° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07858632B2uspto-grants-2010_12