تفاعل #61071

ord-d8cc33e5f25f40949a2c7f8221c44612

معادلة التفاعل

Nc1cc[nH]n1
3-aminopyrazole
O=C([O-])O.[Na+]
NaHCO3
CC(=O)OC(C)=O
Ac2O
CC(=O)Nc1cc[nH]n1
solid
CC(=O)Nc1cc[nH]n1
N-1H-Pyrazol-3-ylacetamide

المتفاعلات

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىat 5-10° C.
  2. 2
    درجة الحرارةThe reaction mixture was refluxed for 8 hr
  3. 3
    workup.WAITwas left
  4. 4
    أخرىcrystallization
  5. 5
    ترشيحThe white solid was filtered (12.9 g)

الإجراء التجريبي

To a solution of 3-aminopyrazole (20 g, 0.24 mol) in H2O (36 mL), at 5-10° C., was slowly added NaHCO3 (9.1 g, mol, 3 eq) and then Ac2O (6.79 ml, 2 eq). The reaction mixture was refluxed for 8 hr. It was cooled down to r.t. and was left standing at this temperature for 12 hr to allow crystallization. The white solid was filtered (12.9 g) and the mother liquor volume was reduced. A second batch of white solid (3.4 g) was obtained after crystallization. The two batches were combined to give the title compound (16.3 g, 54%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07427630B2uspto-grants-2008_09