تفاعل #1605805

ord-2fa158d62ec74a38928f0596082c51e8

معادلة التفاعل

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
المردود 171.2%

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONwere added
  2. 2
    درجة الحرارةthe mixture was heated
  3. 3
    أخرىremoved by a Dean-Stark trap
  4. 4
    تركيزThe reaction solution was concentrated under reduced pressure
  5. 5
    أخرىa solid obtained
  6. 6
    غسيلwas washed with a mixed solvent of hexane-ethyl acetate (4:1)
  7. 7
    ترشيحThe solid was collected by filtration
  8. 8
    أخرىdried under reduced pressure

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09072734B2uspto-grants-2015_07