반응 #55243

ord-fbafb2d7eed545b084420b6dd93457c8

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The mixture is heated at 105°-110° C. for 4 hours
  2. 2
    온도cooled
  3. 3
    추출The product is extracted three times with ether
  4. 4
    기타dried
  5. 5
    농축concentrated on a rotary evaporator
  6. 6
    workup.DISTILLATIONthe residue distilled

실험 절차

Salicylaldehyde (34 g) is treated first with 13.4 g of 50% sodium hydride in 220 ml of dimethylformamide and then with 185 ml of a 2 N toluene solution of N-(2-chloroethyl)morpholine. The mixture is heated at 105°-110° C. for 4 hours, cooled and poured into 300 ml of water. The product is extracted three times with ether. The extracts are combined, dried, concentrated on a rotary evaporator and the residue distilled to give 56.6 g of product as an oil, boiling point 145°-150° C. at 0.05-0.1 mm of Hg.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04151354uspto-grants-1979_04