反応式
Cl.C(O[C:5](=[NH:16])[CH2:6][S:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])=[O:8])C.[OH-].[Na+].C(=O)(O)[O-].[Na+].C[O-].[Na+].I.[NH2:28][C:29]([S:32][CH3:33])=[N:30][NH2:31]>C(Cl)(Cl)Cl.O>[NH2:16][C:5](=[N:31][NH:30][C:29](=[NH:28])[S:32][CH3:33])[CH2:6][S:7]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:9])=[O:8]参加物
反応物 5
生成物 1
試薬・触媒・溶媒 2
実験手順
A suspension of 211 g (0.80 mol) 2-(phenylsulfonyl)-ethanimidic acid ethyl ester hydrochloride in 2 l chloroform was treated with 801 ml 1N aqueous sodium hydoxide. 350 ml of a saturated aqueous sodiumbicarbonate solution was added and the mixture was extracted with chloroform. The extracts were combined and dried with sodium sulfate and the solvents were distilled off under reduced pressure. The resulting oil was dissolved in 450 ml ethanol and the solution was added to a suspension of 44.6 g (0.82 mol) sodiummethylate and 187 g (0.80 mol) methyl aminomethanehydrazonothioate hydroiodide. After 75 minutes at room temperature 4.8 l of a 3/1 water/saturated aqueous sodiumbicarbonate solution was added and the mixture was extracted with chloroform. The organic phase was dried with sodiumsulfate and the solvents were evaporated. Recrystallisation from 1.81 ethanol gave 121 g (53%) 1-[[1-amino-2-(phenylsulfonyl)ethylidene]amino]-2-methyl-2-thiopseudourea (or tautomer), MS m/e (%): 287 (M+H+, 100), 270 (28).
後処理
- extractionthe mixture was extracted with chloroform
- dry with materialdried with sodium sulfate
- distillationthe solvents were distilled off under reduced pressure
- dissolutionThe resulting oil was dissolved in 450 ml ethanol
- extractionthe mixture was extracted with chloroform
- dry with materialThe organic phase was dried with sodiumsulfate
- customthe solvents were evaporated
- customRecrystallisation from 1.81 ethanol
出典と根拠
- ORDレコード
- ord-405a3525525f4c43958550aae1c8409e
- 出典データセット
- uspto-grants-2002_03
- 特許番号
- US06355653B1
関連ノート
読み込み中…