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

HRID 21112

反応式

HRID 21112 の反応式
[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]

参加物

6

反応物 4

HCID 887MethanolHCID 962WaterHCID 13838HexamethyldisilazaneHCID 2820713-Iodophthalic anhydride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-0ee272fea7cd425ebdbaa6a1eccbe4c9
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

関連ノート

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