Iodine → HCID 178432833, 화합물

HRID 1754369노트

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HRID 1754369 반응식
[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]

참가 물질

5

반응물 3

HCID 807IodineHCID 6212ChloroformHCID 178432834HCID 178432834, 화합물

생성물 1

HCID 178432833HCID 178432833, 화합물수율 107.1%

시약·촉매·용매 1

HCID 176Acetic Acid용매

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온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b79a78fc6cc248c9a7bf201f7e8a7dc8
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169248B2

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