تفاعل #969553

ord-f86db14a0f7547e3a6936716e2e6f02b

ظروف التفاعل

درجة الحرارة
-78°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwash
  2. 2
    أخرىgiving a white precipitate
  3. 3
    أخرىThis cold reaction mixture
  4. 4
    ترشيحwas filtered
  5. 5
    أخرىto remove the solid
  6. 6
    تركيزthe filtrate was concentrated to dryness

الإجراء التجريبي

Benzyl 2-aminoacetate was generated from a treatment of benzyl 2-aminoacetate hydrochloride (Aldrich) in methylene chloride with aqueous sodium bicarbonate solution followed by water wash. To a cooled solution of benzyl 2-aminoacetate (1.837 g, 11.1 mmol) and pyridine (1.1 g, 1.1 mL, 13.9 mmol) in methylene chloride (17 mL) at −78° C., was added slowly 1-chloroethyl chloroformate (Aldrich, 1.67 g, 11.7 mmol) over ˜10 min. The reaction mixture was allowed to stir at −78° C. for 3 h, giving a white precipitate. This cold reaction mixture was filtered to remove the solid and the filtrate was concentrated to dryness, giving the crude benzyl 2-((1-chloroethoxy)carbonylamino)acetate which was used for the next step without further purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08993614B2uspto-grants-2015_03