Methylamine → 2-Methylthiophene-3-carboxylic acid
反応式
[Cl-].[CH3:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8]([O-:10])=[O:9].C1COCC1.CN>C(OCC)(=O)C>[CH3:2][C:3]1[S:4][CH:5]=[CH:6][C:7]=1[C:8]([OH:10])=[O:9]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 hydrochloride acid, an aqueous solution of saturated 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 hydrochloride acid, an aqueous solution of saturated 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-543d502e31254f8e811ab60f5ce57690
- 出典データセット
- uspto-grants-2005_04
- 特許番号
- US06875761B2
反応ノート
読み込み中…