Methylamine → n-Methyl-2-methylthiophene-3-carboxamide
反応式
[Cl-].[CH3:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8]([O-:10])=O.C1COCC1.[CH3:16][NH2:17]>C(OCC)(=O)C>[CH3:16][NH:17][C:8]([C:7]1[CH:6]=[CH:5][S:4][C:3]=1[CH3:2])=[O:10]参加物
5
実験手順
2-Methyl-3-thiophenecarboxylate chloride (60.5 g)/THF (300 ml) solution was added dropwise to a 40% aqueous solution of methylamine (400 ml) at 0° C. Ethyl acetate (2 l) was added thereto, and then the organic layer was washed sequentially with water, a 5N aqueous solution of hydrochloric acid, an aqueous solution of saturated sodium bicarbonate, water and brine, dried and evaporated. The resulting residue was crystallized from n-hexane, to give the title compound as a white powder (43.5 g, yield; 71.8%).
後処理
- washthe organic layer was washed sequentially with water
- dry with materiala 5N aqueous solution of hydrochloric acid, an aqueous solution of saturated sodium bicarbonate, water and brine, dried
- customevaporated
- customThe resulting residue was crystallized from n-hexane
出典と根拠
- ORDレコード
- ord-6da2f436209b4808827cb0ddcc1ec0f5
- 出典データセット
- uspto-grants-2002_01
- 特許番号
- US06340759B1
反応ノート
読み込み中…