تفاعل #710478

ord-9eb9c378810042e192573892e1b2cbf6

معادلة التفاعل

Nc1ccccn1
2-aminopyridine
CCN=C=NCCCN(C)C.Cl
EDC-HCl
O=C(O)C(F)(F)C(F)(F)F
pentafluoropropionic acid
O=C(N=c1cccc[nH]1)C(F)(F)C(F)(F)F
2,2,3,3,3-pentafluoro-N-(pyridin-2(1H)-ylidene)propanamide
المردود 11.1%

الكواشف

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    غسيلwashed once with water and twice with 1% hydrochloric acid
  2. 2
    تجفيفdried over anhydrous magnesium sulfate
  3. 3
    تركيزconcentrated under reduced pressure

الإجراء التجريبي

300 mg (3.19 mmol) of 2-aminopyridine was dissolved in 15 ml of anhydrous dichloromethane, 919 mg (4.78 mmol) of EDC-HCl, 583 mg (4.78 mmol) of DMAP and 397 μl (628 mg, 3.83 mmol) of pentafluoropropionic acid were added thereto in sequence, and the resulting mixture was stirred at room temperature overnight. After the reaction was completed, the reaction solution was diluted with dichloromethane, washed once with water and twice with 1% hydrochloric acid, and then dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 85 mg (yield 11%) of 2,2,3,3,3-pentafluoro-N-(pyridin-2(1H)-ylidene)propanamide.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09301525B2uspto-grants-2016_04