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Acetyl chloride → HCID 19349925, 화합물

HRID 1672794
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HRID 1672794 반응식
[OH:1][N:2]=[C:3]([NH2:11])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([I:10])[CH:5]=1.[C:12](Cl)(=O)[CH3:13]>N1C=CC=CC=1.C(OCC)(=O)C>[I:10][C:6]1[CH:5]=[C:4]([C:3]2[N:11]=[C:12]([CH3:13])[O:1][N:2]=2)[CH:9]=[CH:8][CH:7]=1
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참가 물질

5

반응물 2

HCID 6367Acetyl chlorideHCID 44235713-Iodo-N-hydroxy-benzamidine

생성물 1

HCID 19349925HCID 19349925, 화합물수율 39%

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8857Ethyl Acetate용매

실험 절차

N′-Hydroxy-3-iodobenzamidine (1.80 g, 6.87 mmol) obtained in Step 1 was dissolved in pyridine (14 mL), and the mixture was stirred at room temperature for 1 hour after adding acetyl chloride (0.551 mL, 6.87 mmol). The mixture was cooled to room temperature after further stirring at 90° C. for 4 hours. After diluting the mixture with ethyl acetate, the organic layer was washed with 1 mol/L hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate. The residue obtained upon concentration under reduced pressure was then purified by silica gel column chromatography to give 3-(3-iodophenyl)-5-methyl-1,2,4-oxadiazole (756 mg, 39%).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. stirringafter further stirring at 90° C. for 4 hours
  3. washthe organic layer was washed with 1 mol/L hydrochloric acid and saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe residue obtained upon concentration under reduced pressure
  6. customwas then purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-035e42d46afd4f1495ddc3813c4c0acd
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07998954B2

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