반응 #95428

ord-4fda088e904e42a7a0008e495677d659

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction solution is evaporated to dryness
  2. 2
    여과the precipitate is filtered off
  3. 3
    세척washed with water
  4. 4
    workup.DISSOLUTIONdissolved in methylene chloride
  5. 5
    건조After drying over sodium sulphate
  6. 6
    기타evaporating

실험 절차

11 g of 4-chloro-3-nitro-benzophenone, 20 g of methylamine, 153.4 g of methanol and 27.5 g of sulpholane are warmed to 125° for 15 hours in a closed vessel. The reaction solution is evaporated to dryness, the residue is boiled thoroughly with 400 ml of 2 N hydrochloric acid for 20 minutes and the precipitate is filtered off, washed with water and dissolved in methylene chloride. After drying over sodium sulphate and evaporating, 4-methylamino-3-nitro-benzophenone with a melting point of 198°-201° is obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04344957uspto-grants-1982_08