반응 #669908

ord-59cc54f87c6e4be3ad316bb9afee6f32

반응 조건

온도
27.5°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출The resulting solution was extracted with ethyl acetate
  2. 2
    건조The extracts were dried over magnesium sulfate
  3. 3
    여과filtered
  4. 4
    농축concentrated
  5. 5
    기타to give 49.1 g (98%) of the crude material
  6. 6
    기타Recrystallization from 100 ml of ethyl acetate

실험 절차

A mixture of 60 g of ethyl 2-oxobicyclo[3.1.0]hexane-6-carboxylate and 300 ml of 1 N sodium hydroxide was stirred at 25-30° C. After 2.5 hours, concentrated hydrochloric acid was added to adjust the pH to 0.8-1.2. The resulting solution was extracted with ethyl acetate. The extracts were dried over magnesium sulfate, filtered, and concentrated to give 49.1 g (98%) of the crude material. Recrystallization from 100 ml of ethyl acetate gave the title compound, mp 123.5-128° C. FDMS: m/z =140 (M+) Analysis calculated for C7H8O3 : C, 60.00; H, 5.75. Found: C, 60.14; H, 5.79.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05925680uspto-grants-1999_07