반응 #66624

ord-002d85a37465404faed8fd0a486b2a3b

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: US08524725B2uspto-grants-2013_09