Iodine → 3-Amino-4-iodo-6-bromophthalimide

HRID 20996

反応式

HRID 20996 の反応式
[I:1]I.[NH2:3][C:4]1[CH:14]=[CH:13][C:12]([Br:15])=[C:6]2[C:7]([NH:9][C:10](=[O:11])[C:5]=12)=[O:8].S([O-])([O-])(=O)=S.[Na+].[Na+]>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[NH2:3][C:4]1[C:14]([I:1])=[CH:13][C:12]([Br:15])=[C:6]2[C:7]([NH:9][C:10](=[O:11])[C:5]=12)=[O:8]

参加物

6

反応物 3

HCID 807IodineHCID 24477Sodium ThiosulfateHCID 684890894-amino-7-bromo-2,3-dihydro-1H-isoindole-1,3-dione

生成物 1

HCID 684887173-Amino-4-iodo-6-bromophthalimide収率 96%

試薬・触媒・溶媒 2

HCID 178418844HCID 178418844、化合物触媒HCID 702Ethanol溶媒

実験手順

Iodine (6.29 g, 24.8 mmol) was dissolved in ethanol (225 mL), and the solution was added with silver sulfate (3.87 g, 12.4 mmol) and 3-amino-6-bromophthalimide (3.00 g, 12.4 mmol), followed by stirring at room temperature for 23 hours. The reaction mixture was added with 10% aqueous sodium thiosulfate solution and extracted with ethyl acetate. The organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, the residue was purified by slurry using hexane and methanol to obtain 3-amino-4-iodo-6-bromophthalimide (4.3 g. yield 96%).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with 0.5 mol/L hydrochloric acid and saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customthe residue was purified by slurry

出典と根拠

ORDレコード
ord-7387e8246d2a488ebc482fbdeadd6168
出典データセット
uspto-grants-2010_06
特許番号
US07745641B2

関連ノート

読み込み中…