반응 #502106

ord-9738909b5b2b4a118505adb3bac6ad7f

반응 방정식

O=C(O)c1n[nH]c2ccccc12
1H-indazole-3-carboxylic acid
CNOC.Cl
N,O-dimethylhydroxylamine hydrochloride
CCN=C=NCCCN(C)C
1-(3-dimethylaminopropyl)-3-ethylcarbodiimide
c1ccncc1
pyridine
CON(C)C(=O)c1n[nH]c2ccccc12
compound
수율 69.1%
CON(C)C(=O)c1n[nH]c2ccccc12
N-Methoxy-N-methyl-1H-indazole-3-carboxamide
수율 69.1%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The mixture is concentrated
  2. 2
    기타The yellow precipitate obtained
  3. 3
    세척is washed with water
  4. 4
    기타dried under reduced pressure

실험 절차

In a round-bottomed flask, 4.0 g of 1H-indazole-3-carboxylic acid, 2.6 g of N,O-dimethylhydroxylamine hydrochloride, 9.4 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and 8.4 ml of pyridine are placed in 120 ml of tetrahydrofuran. The mixture is stirred at ambient temperature for 20 h. The mixture is concentrated and the residue is taken up in water. The yellow precipitate obtained is washed with water and then dried under reduced pressure. 3.5 g of compound are obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08088765B2uspto-grants-2012_01