N-Iodosuccinimide → HCID 178432833, 화합물

HRID 1488091노트

반응식

HRID 1488091 반응식
[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]

참가 물질

5

반응물 2

HCID 120273N-IodosuccinimideHCID 178432834HCID 178432834, 화합물2회

생성물 1

HCID 178432833HCID 178432833, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-095f6a4879a741afaa329ab33dbb6185
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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