반응 #1605805

ord-2fa158d62ec74a38928f0596082c51e8

반응 방정식

Nc1cc(CCCC(=O)O)ccc1-c1ccccc1
4-(3-Amino-4-phenylphenyl)butyric acid
Cc1ccc(S(=O)(=O)O)cc1.O
tosylic acid hydrate
O
water
Cc1ccc(S(=O)(=O)O)cc1.Nc1cc(CCCC(=O)OCc2ccccc2)ccc1-c1ccccc1
benzyl 4-(3-amino-4-phenylphenyl)butyrate tosylate
수율 171.2%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONwere added
  2. 2
    온도the mixture was heated
  3. 3
    기타removed by a Dean-Stark trap
  4. 4
    농축The reaction solution was concentrated under reduced pressure
  5. 5
    기타a solid obtained
  6. 6
    세척was washed with a mixed solvent of hexane-ethyl acetate (4:1)
  7. 7
    여과The solid was collected by filtration
  8. 8
    기타dried under reduced pressure

실험 절차

To a suspension of 4-(3-Amino-4-phenylphenyl)butyric acid (21.6 g, 84.6 mmol) in toluene (300 mL), benzyl alcohol (50 mL) and tosylic acid hydrate (17.7 g, 93.0 mmol) were added, and the mixture was heated under reflux for 5 hours with water removed by a Dean-Stark trap. The reaction solution was concentrated under reduced pressure and a solid obtained was washed with a mixed solvent of hexane-ethyl acetate (4:1). The solid was collected by filtration and dried under reduced pressure to obtain benzyl 4-(3-amino-4-phenylphenyl)butyrate tosylate (41.2 g).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09072734B2uspto-grants-2015_07