N-Iodosuccinimide → HCID 178432833、化合物

HRID 1488091ノート

反応式

HRID 1488091 の反応式
[CH3:1][C:2]1[NH:3][CH:4]=[C:5]([C:7]([F:10])([F:9])[F:8])[N:6]=1.C1C(=O)N([I:18])C(=O)C1>CC#N.O>[I:18][C:4]1[NH:3][C:2]([CH3:1])=[N:6][C:5]=1[C:7]([F:10])([F:9])[F:8]

参加物

5

反応物 2

HCID 120273N-IodosuccinimideHCID 178432834HCID 178432834、化合物2 回

生成物 1

HCID 178432833HCID 178432833、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

Into a 50-mL round-bottom flask, was placed a solution of 2-methyl-4-(trifluoromethyl)-1H-imidazole (compound 16.2, 1.72 g, 11.46 mmol) in CH3CN (25 mL). NIS (3.87 g, 17.20 mmol) was added to the reaction. The reaction mixture was stirred overnight at 85. The reaction mixture diluted with 50 mL of H2O and extracted with 3×30 mL of ethyl acetate. The combined organic layers were washed with 2×20 mL of Na2S2O3(sat.) and 2×20 mL of brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. This resulted in 4.32 g (crude) of the title compound as a brown oil.

後処理

  1. customInto a 50-mL round-bottom flask, was placed
  2. extractionextracted with 3×30 mL of ethyl acetate
  3. washThe combined organic layers were washed with 2×20 mL of Na2S2O3(sat.) and 2×20 mL of brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-095f6a4879a741afaa329ab33dbb6185
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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