反応 #502106

ord-9738909b5b2b4a118505adb3bac6ad7f

反応方程式

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
収率 69.1%
CON(C)C(=O)c1n[nH]c2ccccc12
N-Methoxy-N-methyl-1H-indazole-3-carboxamide
収率 69.1%

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The mixture is concentrated
  2. 2
    その他The yellow precipitate obtained
  3. 3
    洗浄is washed with water
  4. 4
    その他dried under reduced pressure

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08088765B2uspto-grants-2012_01