반응 #62721

ord-27c1df14c2bf48e0966f9cafb3f8d0c3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과filtered
  2. 2
    기타evaporated to dryness
  3. 3
    기타Further drying at 40° C. in a vacuum oven

실험 절차

To 2,4-diamino-5-(7,8-dimethoxy-2H-1-benzopyran-5-ylmethyl)pyrimidine (5.00 g, 15.9 mmol) in 450 mL of boiling methanol was added a solution of citric acid monohydrate (3.34 g, 15.9 mmol) in 50 mL of methanol. The solution was treated with charcoal, filtered, and evaporated to dryness. Further drying at 40° C. in a vacuum oven gave 8.01 g (99.5%) of the title compound. Karl Fisher analysis: 5.3% H2O. Anal. Calcd for C16H18N4O3.C6H8O7.1.5H2O: C, 49.53; H, 5.48; N, 10.50. Found: C, 49.54; H, 5.49; N, 10.47.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04761475uspto-grants-1988_08