반응 #50437

ord-e000064620014360bd4ff23c9d507bc0

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도at reflux temperature
  2. 2
    농축Concentration
  3. 3
    여과the resulting crystals are filtered off
  4. 4
    세척washed with water

실험 절차

15.2 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-methoxyphthalide (see Example 8) are heated at reflux temperature in a 1:1 mixture of tetrahydrofuran and hydrochloric acid for 3 hours. Concentration is then carried out under reduced pressure and the resulting crystals are filtered off and washed with water to yield pure 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide, m.p. 143°-145° C.; IR (KBr): 1770 cm-1 ; 1H-NMR (CDCl3): 6.60 ppm (s, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05428002uspto-grants-1995_06