Iodine → HCID 178432833、化合物

HRID 1754369ノート

反応式

HRID 1754369 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.C(Cl)(Cl)Cl.[I:15]I>CC(O)=O>[I:15][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 3

HCID 807IodineHCID 6212ChloroformHCID 178432834HCID 178432834、化合物

生成物 1

HCID 178432833HCID 178432833、化合物収率 107.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

To 2-methyl-4-(trifluoromethyl)-1H-imidazole (1 g, 6.7 mmol) was added CHCl3 (4.5 mL) and AcOH (13.5 mL) followed by I2 (1.78 g, 6.99 mmol) and HIO4.2H2O (1.52 g, 6.7 mmol), and the resulting reaction mixture was stirred at 60° C. for 3 h. The reaction mixture was then poured into ice cold 10% aqueous sodium bisulphite solution (100 mL) and the aqueous layer was extracted with EtOAc (3×100 mL). The combined organic layers were washed with brine (100 mL), dried (MgSO4) and concentrated in vacuo to obtain 5-iodo-2-methyl-4-(trifluoromethyl)-1H-imidazole (1.98 g) which was used as such in next step without further purification.

後処理

  1. customthe resulting reaction mixture
  2. extractionthe aqueous layer was extracted with EtOAc (3×100 mL)
  3. washThe combined organic layers were washed with brine (100 mL)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-b79a78fc6cc248c9a7bf201f7e8a7dc8
出典データセット
uspto-grants-2015_10
特許番号
US09169248B2

反応ノート

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