反応 #2161250

ord-23bc4e7f17454e83900db210da16f2fe

反応方程式

CCOC(=O)c1nc([N+](=O)[O-])c[nH]1
ethyl 4-nitro-1H-imidazole-2-carboxylate
BrCC1CC1
cyclopropylmethyl bromide
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CCOC(=O)c1nc([N+](=O)[O-])cn1CC1CC1
Ethyl 1-(cyclopropylmethyl)-4-nitro-1H-imidazole-2-carboxylate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度After cooling
  2. 2
    抽出extracted four times with ethyl acetate
  3. 3
    洗浄The combined organic phases are washed once with water and three times with a saturated sodium chloride solution
  4. 4
    乾燥dried with magnesium sulfate
  5. 5
    濃縮concentrated in vacuo
  6. 6
    その他The crystalline residue is directly used further for the next reaction

実験手順

Under argon, 15 g (81 mmol) of ethyl 4-nitro-1H-imidazole-2-carboxylate are stirred with 13.13 g (97.2 mmol) of cyclopropylmethyl bromide and 22.4 g (162 mmol) of potassium carbonate in 165 ml of DMF at 80° C. for 1 h. After cooling, the reaction mixture is diluted with water and extracted four times with ethyl acetate. The combined organic phases are washed once with water and three times with a saturated sodium chloride solution, dried with magnesium sulfate and concentrated in vacuo. The crystalline residue is directly used further for the next reaction.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07919489B2uspto-grants-2011_04