반응 #169202

ord-e3eb65687a5b40aca63272abc8d1d7f7

반응 조건

온도
85°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도then cooled to room temperature
  2. 2
    여과filtered
  3. 3
    세척The precipitate was washed with water
  4. 4
    기타dried

실험 절차

To a solution of 3-aminopyrazole (224 g, 2.7 mol) in water (1 L) were added a solution of diethyl oxalacetate sodium salt (567 g, 2.7 mol) in water (1.3 L) and then acetic acid in 4 portions (0.8 L). The reaction mixture was heated at 85° C. for 15 hours then cooled to room temperature and filtered. The precipitate was washed with water and then dried to afford the title compound as an orange solid (159 g, 28%). 1H NMR (250 MHz, DMSO): δ 1.35 (t, 3H), 4.36 (q, 2H), 6.69 (s, 1H), 8.16 (s, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08846712B2uspto-grants-2014_09