Water → 6-iodo-2H-3,1-benzoxazine-2,4(1H)-dione
反応式
[I:1][C:2]1[CH:3]=[CH:4][C:5]([NH2:11])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].[C:12](=O)([O-])[O-:13].[Na+].[Na+].O.C(Cl)(Cl)=O>C1(C)C=CC=CC=1>[I:1][C:2]1[CH:10]=[C:6]2[C:7]([O:9][C:12](=[O:13])[NH:11][C:5]2=[CH:4][CH:3]=1)=[O:8]参加物
6
実験手順
To a mechanically stirred solution of 26.3 grams of 5-iodo-2-amino benzoic acid (0.1 mol), 10.6 grams of sodium carbonate (0.1 mol), and 250 mL water, cooled to 0° C., was slowly added, via an addition funnel, 80 mL of a 1.93M solution of phosgene in toluene. After 2 hours, the precipitated product was isolated by filtration. The solids were washed with 200 mL water, 300 mL of a 1:1 mixture ethanol and ether, 200 mL of ether, and dried under vacuum to yield 24.3 grams (84%) of 5-iodoisatoic anhydride (264°-268° C., decomposition).
後処理
- additionwas slowly added, via an addition funnel
- customthe precipitated product was isolated by filtration
- washThe solids were washed with 200 mL water, 300 mL of a 1:1 mixture ethanol and ether, 200 mL of ether
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-c88da46492a14f20ab06712d2817ee37
- 出典データセット
- uspto-grants-1997_10
- 特許番号
- US05674865
反応ノート
読み込み中…