Methanol → 4-iodo-1H-Isoindole-1,3(2H)-dione

HRID 21112

반응식

HRID 21112 반응식
[I:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:4]2[C:5]([O:7][C:8](=O)[C:3]=12)=[O:6].C[Si](C)(C)[NH:15][Si](C)(C)C.CO.O>CN(C=O)C>[I:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:4]2[C:5]([NH:15][C:8](=[O:7])[C:3]=12)=[O:6]

참가 물질

6

반응물 4

HCID 887MethanolHCID 962WaterHCID 13838HexamethyldisilazaneHCID 2820713-Iodophthalic anhydride

생성물 1

HCID 184075124-iodo-1H-Isoindole-1,3(2H)-dione수율 68%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

3-Iodophthalic anhydride (598 mg, 2.18 mmol) was dissolved in DMF (14 mL), and the solution was added with an aqueous solution (10 mL) of hexamethyldisilazane (HMDS) (4.6 mL, 22 mmol) and methanol (0.44 mL, 11 mmol), followed by stirring at room temperature for 18.5 hours. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure a and the residue was purified by slurry using chloroform to obtain 3-iodophtalimide (403 mg, yield 68%).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure a and the residue
  5. customwas purified by slurry

출처 및 근거

ORD 기록
ord-0ee272fea7cd425ebdbaa6a1eccbe4c9
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745641B2

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