Methylamine → methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate
反応式
Cl[S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3].C1COCC1.[CH3:19][NH2:20]>C(Cl)Cl>[CH3:19][NH:20][S:2]([C:5]1[CH:9]=[CH:8][S:7][C:6]=1[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3]参加物
5
実験手順
To a solution of methyl 3-(chlorosulfonyl)thiophene-2-carboxylate (500 mg, 2.077 mmol) in DCM (20 ml), methanamine 2N solution in THF (4.155 ml, 8.31 mmol) was added and the reaction was stirred for 1 hour at RT. The mixture was partitioned between 2N HCl and DCM and the aqueous phase was extracted with DCM. The combined organic layers were dried over sodium sulfate and the solvent was removed affording methyl 3-(N-methylsulfamoyl)thiophene-2-carboxylate (Int. 32) (430 mg, 1.828 mmol, MS/ESI+235.8 [MH]+).
後処理
- customThe mixture was partitioned between 2N HCl and DCM
- extractionthe aqueous phase was extracted with DCM
- dry with materialThe combined organic layers were dried over sodium sulfate
- customthe solvent was removed
出典と根拠
- ORDレコード
- ord-9b66d920a79c456da03aea4e17f10758
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09440954B2
反応ノート
読み込み中…