反応式
Cl.[N+:2]([C:5]1[CH:6]=[C:7]([C:11]2[N:12]=[C:13]([NH2:16])[S:14][CH:15]=2)[CH:8]=[CH:9][CH:10]=1)([O-:4])=[O:3].[CH3:17][O:18][C:19]1[CH:24]=[CH:23][C:22]([S:25](Cl)(=[O:27])=[O:26])=[CH:21][CH:20]=1.Cl>N1C=CC=CC=1>[CH3:17][O:18][C:19]1[CH:20]=[CH:21][C:22]([S:25]([NH:16][C:13]2[S:14][CH:15]=[C:11]([C:7]3[CH:8]=[CH:9][CH:10]=[C:5]([N+:2]([O-:4])=[O:3])[CH:6]=3)[N:12]=2)(=[O:27])=[O:26])=[CH:23][CH:24]=1参加物
実験手順
A mixture of 0.5 g of 4-(3-nitro-phenyl)-thiazol-2-ylamine hydrochloride with 0.44 g of 4-methoxybenzenesulfonyl chloride was stirred overnight with 2 ml of pyridine. The resulting, red colored suspension was poured into 50 ml of 1N hydrochloric acid and the solid which thereby separated was filtered off and dissolved in a mixture of 40 ml of ethanol and 20 ml of 2N sodium hydroxide solution. After the addition of 0.5 g of active charcoal the mixture was stirred at room temperature for 30 minutes and subsequently the active charcoal was filtered off. The product separated upon neutralization with concentrated hydrochloric acid. Recrystallization from 40 ml of 50% ethanol yielded 0.31 g of 4-methoxy-N-[4-(3-nitro-phenyl)-thiazol-2-yl]-benzenesulfonamide as yellowish crystals.
後処理
- customthe solid which thereby separated
- filtrationwas filtered off
- dissolutiondissolved in a mixture of 40 ml of ethanol and 20 ml of 2N sodium hydroxide solution
- additionAfter the addition of 0.5 g of active charcoal the mixture
- filtrationsubsequently the active charcoal was filtered off
- customThe product separated upon neutralization with concentrated hydrochloric acid
- customRecrystallization from 40 ml of 50% ethanol
出典と根拠
- ORDレコード
- ord-d68b9036e689405eaf15e25edf03e001
- 出典データセット
- uspto-grants-1999_03
- 特許番号
- US05877193
関連ノート
読み込み中…