반응 #50443

ord-5db9dc541d104704a857d69cebb76a01

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONthe whole is treated dropwise at from -7° to -3° C.
  2. 2
    기타the crystals which have separated
  3. 3
    여과are then filtered off
  4. 4
    세척They are washed with water
  5. 5
    기타recrystallised from acetone/n-hexane

실험 절차

1.0 g of 7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-3-hydroxy-phthalide (see Example 84) is introduced into a solution of 2.1 g of potassium cyanide in 15 ml of water and the whole is treated dropwise at from -7° to -3° C., with cooling, over a period of 10 minutes, with 10 ml of concentrated hydrochloric acid. It is subsequently stirred at room temperature for approximately 16 hours and the crystals which have separated are then filtered off. They are washed with water and recrystallised from acetone/n-hexane to yield 0.2 g of 3-carbamoyl-7-[(4,6-dimethoxy-pyrimidin-2-yl)oxy]-phthalide (see also Example 17).

출처

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