HRID1835134

反应详情

EQUATION

反应方程式

HRID 1835134 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Methyl 4-(3-methyl-1-oxobutyl)-1-(1-naphthalenylmethyl)-1H-pyrrole-3-carboxylate (0.35 g) prepared as described in c) above and methylhydrazine (0.10 ml) in ethanol (15 ml) were heated to reflux for 16 hours. The mixture was poured into dilute hydrochloric acid and extracted with ethyl acetate, which was washed with brine, dried, and evaporated to a gum. The gum was chromatographed with ethyl acetate-isohexane (1:1) to afford a solid which was recrystallised from cyclohexane to give 2,6-dihydro-2-methyl-4-(2-methylpropyl)-6-(1-naphthalenylmethyl)-1H-pyrrolo[3,4-d]pyridazin-1-one (0.16 g).

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureto reflux for 16 hours
  3. extractionextracted with ethyl acetate, which
  4. washwas washed with brine
  5. customdried
  6. customevaporated to a gum
  7. customThe gum was chromatographed with ethyl acetate-isohexane (1:1)
  8. customto afford a solid which
  9. customwas recrystallised from cyclohexane