반응 #4889

ord-b804369893e54bd59770ee9a23839cc6

시약

없음

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타slowly rose to 50° C
  2. 2
    온도After 0.5 hr the stirred mixture was heated
  3. 3
    온도to reflux
  4. 4
    기타the water was collected in a Dean-Stark trap for 48 hours
  5. 5
    기타A total of 93 ml of water was collected
  6. 6
    workup.ADDITIONThe toluene residue was treated with 300 ml of ethanol
  7. 7
    농축concentrated on the rotary evaportor
  8. 8
    workup.DISTILLATIONThe residue was distilled
  9. 9
    기타The yield of product obtained
  10. 10
    기타145°/0.5 mm

실험 절차

To a stirred solution of 134 g (1 mole) of (S)-malic acid in 700 ml of toluene was added 97 ml of 40% aqueous methylamine. The temperature slowly rose to 50° C. After 0.5 hr the stirred mixture was heated to reflux and the water was collected in a Dean-Stark trap for 48 hours. A total of 93 ml of water was collected. The toluene residue was treated with 300 ml of ethanol and concentrated on the rotary evaportor. The residue was distilled. The yield of product obtained was 101 g (78%), b.p. 140°/2 mm; 145°/0.5 mm.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04727152uspto-grants-1988_02