تفاعل #1969502

ord-2acca6be9521485bbd69f060c81abbb2

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىfor 30 minutes
  2. 2
    ترشيحThe catalyst was filtered
  3. 3
    تركيزthe filtrate concentrate hexane (3 mL)
  4. 4
    workup.ADDITIONadded
  5. 5
    ترشيحfiltered solid

الإجراء التجريبي

[2-(4-Nitrophenoxy)-ethoxy]acetic acid methyl ester 74 (1 grams, 3.9 mmol) was dissolved in anhydrous ethyl acetate (20 mL), palladium carbon (10%, 0.1 gram) added and the mixture stirred under an atmosphere of H using balloon for 30 minutes. The catalyst was filtered, the filtrate concentrate hexane (3 mL) added, filtered solid to give 75 (625 mg, 70.9%) as a light brown powder. The melting point was found to be 51-52.5° C. The structure was confirmed with IR and NMR. IHNMR (CDCl3) 3.04 (bs, 2H, NH2), 3.72 (s, 3H, ester), 3.88 (t, 2H, OCH2), 4.08 (t, 2H, OCH2), 4.20 (s, 2H, OCH2), 6.58 (d, 2H, Ar), 6.70 (d, 2H, Ar).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08318973B2uspto-grants-2012_11