反応式
N[C:2]1[C:10]2S[N:8]=[CH:7][C:6]=2[CH:5]=[C:4]([N+:11]([O-:13])=[O:12])[CH:3]=1.S(=O)(=O)(O)O.P(=O)(O)(O)O.[N:24](OS(=O)(=O)O)=O.[CH:31]([O:33][C:34](=[O:46])[CH2:35][CH2:36][N:37]([CH2:44][CH3:45])[C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)=[CH2:32].[S:47](=O)(=O)(O)[NH2:48]>CO>[CH:31]([O:33][C:34](=[O:46])[CH2:35][CH2:36][N:37]([CH2:44][CH3:45])[C:38]1[CH:43]=[CH:42][C:41]([N:24]=[N:8][C:7]2[S:47][N:48]=[C:10]3[CH:2]=[CH:3][C:4]([N+:11]([O-:13])=[O:12])=[CH:5][C:6]=23)=[CH:40][CH:39]=1)=[CH2:32]参加物
反応物 6
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 60 °C
実験手順
5.9 parts of 7-amino-5-nitrobenzisothiazole, 30 parts of 98% sulfuric acid and 8 parts of 85% phosphoric acid were charged, heated at 60° C. for 30 mins, then cooled to 5° C. 11.4 parts of 40% (w/w) nitrosyl sulfuric acid were added, whilst the temperature was held below 10° C. The diazotization mixture was stirred for a further 2 hrs at 5-10° C. To a separate vessel were charged 6.5 parts of 3-(ethyl-phenyl-amino)-propionic acid vinyl ester, 100 parts of methanol, 1 part sulfamic acid and 100 parts of ice. With stirring, the diazotization mixture was slowly added followed by a further 300 parts of ice. The reaction mixture was stirred over night and the product was isolated by filtration, washed with water and dried to yield 10.1 parts of 3-{ethyl-[4-(5-nitro-benzo[c]isothiazol-3-ylazo)-phenyl]-amino}-propionic acid vinyl ester. λmax=606 nm (DMF).
後処理
- temperaturecooled to 5° C
- customwas held below 10° C
- stirringWith stirring
- additionthe diazotization mixture was slowly added
- stirringThe reaction mixture was stirred over night
- customthe product was isolated by filtration
- washwashed with water
- customdried
出典と根拠
- ORDレコード
- ord-a91548c9c95d4b949953dc810420b30e
- 出典データセット
- uspto-grants-2011_01
- 特許番号
- US07871446B2
関連ノート
読み込み中…