Trichloroacetonitrile → 3-{4-[2,4-bis(trichloromethyl)-s-triazine-6-yl]phenyl thio}propionic Acid
反応式
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([S:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[CH:5][CH:4]=1)#[N:2].[Br-].[Br-].[Br-].[Al+3].[Cl:19][C:20]([Cl:24])([Cl:23])[C:21]#[N:22]>>[Cl:19][C:20]([Cl:24])([Cl:23])[C:21]1[N:22]=[C:21]([C:20]([Cl:24])([Cl:23])[Cl:19])[N:22]=[C:1]([C:3]2[CH:4]=[CH:5][C:6]([S:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[CH:7][CH:8]=2)[N:2]=1参加物
4
実験手順
A solution containing 22 g of 3-(4-cyanophenylthio) propionic acid (106 mmol) and 2 g of aluminum tribromide (AlBr3) in 150 g of trichloroacetonitrile was dried at room temperature and bubbled with HCl. The solution was heated with a heat-gun in order to dissolve the starting materials remaining undissolved. The process of reaction was checked by TLC. The reaction product was formed gradually with the lapse of time. Then, the reaction was quenched after 24 hours and the reaction mixture was extracted with 1000 mL of diethyl ether. The resultant product was washed with deionized water and dried over anhydrous magnesium sulfate.
後処理
- customwas dried at room temperature
- custombubbled with HCl
- temperatureThe solution was heated with
- temperaturea heat-gun in order
- dissolutionto dissolve the starting materials
- customThe process of reaction
- customThe reaction product was formed gradually with the lapse of time
- customThen, the reaction was quenched after 24 hours
- extractionthe reaction mixture was extracted with 1000 mL of diethyl ether
- washThe resultant product was washed with deionized water
- dry with materialdried over anhydrous magnesium sulfate
出典と根拠
- ORDレコード
- ord-57398dd6e6574f238fac197d343ea13c
- 出典データセット
- uspto-grants-2015_10
- 特許番号
- US09152041B2
反応ノート
読み込み中…