反応 #11995

反応方程式

(4-amino-3-chloro-5-trifluoromethyl-phenyl)-ethylene oxide

tert-butylamine

→

2-(4-amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol

収率 20.0%

溶媒

ethanol

反応条件

後処理

1. 1
   温度The mixture was refluxed for 13 h
2. 2
   その他evaporated
3. 3
   抽出The residue was extracted with 2N hydrochloric acid for several times
4. 4
   抽出extracted with toluene
5. 5
   workup.ADDITIONtreated with activated carbon
6. 6
   ろ過The precipitate was collected by filtration

実験手順

5.2 g (0.022 mol) of (4-amino-3-chloro-5-trifluoromethyl-phenyl)-ethylene oxide was dissolved in 26 ml of anhydrous ethanol and treated with 5.1 ml (0.049 mol) of tert-butylamine. The mixture was refluxed for 13 h, and then evaporated. The residue was extracted with 2N hydrochloric acid for several times. Aqueous layers were combined and extracted with toluene and treated with activated carbon. The pH was adjusted to 10 with 20% sodium hydroxide solution. The precipitate was collected by filtration, 2-(4-amino-3-chloro-5-trifluoromethylphenyl)-2-tert-butylaminoethanol was obtained. Yield 20–30%; melting point 85–90° C.

出典