Methyl 5-amino-o-anisate → Methyl5-isothiocyanato-2-methoxybenzoate
反応式
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6].C1C=C(O[C:21](OC2N=CC=CC=2)=[S:22])N=CC=1>ClCCl>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]([N:13]=[C:21]=[S:22])=[CH:9][C:4]=1[C:5]([O:7][CH3:8])=[O:6]参加物
4
実験手順
According to the method of Tet. Let., 26, 1661 (1985), combine methyl 2-methoxy-5-aminobenzoate (0.5 g, 2.76 mmol) and di-2-pyridyl thionocarbonate (0.64 g, 2.76 mmol) in dichloromethane (10 mL). After 30 minutes, dilute the reaction mixture with dichloromethane and extract five times with water. Dry the organic layer over Na2SO4, filter, and concentrate in vacuo to give methyl 2-methoxy-5-thioisocyanatobenzoate: Rf=0.51 (silica gel, dichloromethane).
後処理
- extractionextract five times with water
- dry with materialDry the organic layer over Na2SO4
- filtrationfilter
- concentrationconcentrate in vacuo
出典と根拠
- ORDレコード
- ord-49b52d5f51374e28acdfc541cf98a2de
- 出典データセット
- uspto-grants-2001_04
- 特許番号
- US06211199B1
反応ノート
読み込み中…