تفاعل #1909792

ord-f6af6587c2b6444a802684fc0cce1da6

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThen, the obtained reaction mixture
  2. 2
    استخلاصwas extracted with dichloromethane
  3. 3
    تجفيفthe organic layer was dried over anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONThereafter, the solvent was distilled off under reduced pressure
  5. 5
    أخرىthe resultant residue was subjected to re-crystallization treatment
  6. 6
    ترشيحwas subjected to a suction filtration

الإجراء التجريبي

2.47 g (0.007 mol) of N-[(9-fluorenyl)methoxycarbonyl]-L-isoleucine, 1.89 g (0.007 mol) of octadecylamine, 85.5 mg (0.0007 mol) of 4-(N,N-dimethylamino)pyridine (DMAP), and 1.61 g (0.0084 mol) of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC) was dissolved in 45 ml of dichloromethane, and the resultant solution was stirred for 4 days at room temperature. Then, the obtained reaction mixture was extracted with dichloromethane, and the organic layer was dried over anhydrous magnesium sulfate. Thereafter, the solvent was distilled off under reduced pressure, the resultant residue was subjected to re-crystallization treatment using ethyl acetate, and gel-like substance was subjected to a suction filtration, thereby obtaining 3.69 g of N-[(9-fluorenyl)methoxycarbonyl]-L-isoleucylaminooctadecane (hereinafter also referred to as “Intermediate product (1)”) at the yield of 87%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07037444B2uspto-grants-2006_05