Ammonia → HCID 67274431、化合物
反応式
[CH3:1][O:2][CH2:3][CH2:4][C:5]1[S:9][C:8]([S:10](Cl)(=[O:12])=[O:11])=[CH:7][C:6]=1[CH3:14].[NH3:15]>CC(C)=O>[CH3:1][O:2][CH2:3][CH2:4][C:5]1[S:9][C:8]([S:10]([NH2:15])(=[O:12])=[O:11])=[CH:7][C:6]=1[CH3:14]参加物
4
実験手順
To a solution of 1.40 g (55 mM) 5-(2-methoxy-ethyl)-4-methyl-thiophene-2-sulfonyl chloride in 20 ml acetone was added 5 ml of an aqueous solution of ammonia (25%) and the mixture was stirred at room temperature for 1 h. The mixture was partitioned between water and ethyl acetate. The phases were separated and the organic phase was dried over sodium sulfate and evaporated. The residue purified by chromatography on silica gel crystallized form cyclohexane/diethyl ether to yield 0.89 g of the title compound as light red solid. MS (ISN) M−H+=233.8
後処理
- customThe mixture was partitioned between water and ethyl acetate
- customThe phases were separated
- dry with materialthe organic phase was dried over sodium sulfate
- customevaporated
- customThe residue purified by chromatography on silica gel
- customcrystallized
- customform cyclohexane/diethyl ether
出典と根拠
- ORDレコード
- ord-a2609e74dd6d4de7b4539492bf744c33
- 出典データセット
- uspto-grants-2012_04
- 特許番号
- US08163778B2
反応ノート
読み込み中…