反応式
N[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12].OS(O)(=O)=O.N([O-])=O.[Na+].[Na+].[I-:25]>O>[I:25][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[C:11]([F:14])([F:13])[F:12]参加物
6
実験手順
To a mixture of 3.1 g (15.0 mmol) of 2-amino-5-nitrobenzotrifluoride in 60 mL of 40% (v/v) H2SO4 stirred in an ice-bath was added dropwise a solution of 2.1 g (30.4 mmol) of NaNO2 in 10 mL of H2O. The resulting yellow solution was stirred in an ice-bath for 1 h and it was added dropwise into a well stirred solution of 10 g of NaI in 250 mL of H2O cooled in an ice bath. Gas releasing and precipitate was observed. The mixture was stirred overnight at 25° C., filtered and washed by water, and dried to leave pale yellow solid (4.5 g, 94%), mp 81°-82° C. 1H NMR (CDCl3), 8.047 (dd, 1), 8.272 (d, 1), 8.483 (d, 1).
後処理
- stirringThe resulting yellow solution was stirred in an ice-bath for 1 h
- additionit was added dropwise into a well
- temperaturecooled in an ice bath
- stirringThe mixture was stirred overnight at 25° C.
- filtrationfiltered
- washwashed by water
- customdried
出典と根拠
- ORDレコード
- ord-927e014c875c4451a486c552d6849f30
- 出典データセット
- uspto-grants-1997_04
- 特許番号
- US05622952
関連ノート
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