Cyanogen Bromide → 6-(Methanesulfonyl)-1H-benzimidazol-2-amine
反応式
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH2:11])=[C:7]([NH2:12])[CH:6]=1)(=[O:4])=[O:3].[N:13]#[C:14]Br>O>[NH2:13][C:14]1[NH:12][C:7]2[CH:6]=[C:5]([S:2]([CH3:1])(=[O:3])=[O:4])[CH:10]=[CH:9][C:8]=2[N:11]=1参加物
4
実験手順
One mole, 186.1 g., of 4-methylsulfonyl-o-phenylenediamine was suspended in 1.2 l. of water with stirring. One mole, 106 g., of cyanogenbromide was added portionwise to the reaction mixture. The reaction mixture was stirred for 4 hours and then filtered. Sodium hydroxide, 39 g. (1 m.) in 500 ml. of water, was added to the filtrate. The aqueous mixture was cooled in an ice bath and the product crystallized. The product was collected and dried before crystallization from ethanol-ether; yield 200 g., m.p. 233°-238° C.
後処理
- filtrationfiltered
- additionof water, was added to the filtrate
- temperatureThe aqueous mixture was cooled in an ice bath
- customthe product crystallized
- customThe product was collected
- dry with materialdried before crystallization from ethanol-ether
出典と根拠
- ORDレコード
- ord-01280097e53f4ab884f9ec05f9d9ee2b
- 出典データセット
- uspto-grants-1978_10
- 特許番号
- US04118573
反応ノート
読み込み中…