Triethylamine → HCID 20229919、化合物
反応式
[OH:1][CH:2]1[CH2:6][CH2:5][O:4][CH2:3]1.C(N(CC)CC)C.[C:14]([C:16]1[CH:24]=[CH:23][C:22]([O:25][C:26]2[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:27]=2[Cl:33])=[CH:21][C:17]=1[C:18](Cl)=[O:19])#[N:15]>C1(C)C=CC=CC=1>[C:14]([C:16]1[CH:24]=[CH:23][C:22]([O:25][C:26]2[CH:31]=[CH:30][C:29]([Cl:32])=[CH:28][C:27]=2[Cl:33])=[CH:21][C:17]=1[C:18]([O:1][CH:2]1[CH2:6][CH2:5][O:4][CH2:3]1)=[O:19])#[N:15]参加物
実験手順
3-Hydroxytetrahydrofuran (0.04 mole), toluene (50 ml) and triethylamine (0.04 mole) are charged into a glass reaction vessel equipped with a mechanical stirrer and addition funnel. A solution of 2-cyano-5-(2,4-dichlorophenoxy)benzoyl chloride (0.04 mole) in toluene (20 ml) is slowly added at room temperature with stirring. After the addition is completed, stirring is continued for a period of about eight hours. After this time, the reaction mixture is washed with water and dried over anhydrous magnesium sulfate. The dried solution is then stripped of solvent under reduced pressure leaving a residue. This residue is purified by silica gel chromatography using toluene and ethyl acetate/toluene mixture as the eluant to yield the desired product 3-tetrahydrofuryl 2-cyano-5-(2,4l -dichlorophenoxy)benzoate.
後処理
- customequipped with a mechanical stirrer and addition funnel
- additionAfter the addition
- stirringstirring
- washAfter this time, the reaction mixture is washed with water
- dry with materialdried over anhydrous magnesium sulfate
- customleaving a residue
- customThis residue is purified by silica gel chromatography
出典と根拠
- ORDレコード
- ord-bba52bd40bdc4aaf804e3c8882e1f62a
- 出典データセット
- uspto-grants-1986_10
- 特許番号
- US04618359
反応ノート
読み込み中…