反応 #1366

反応方程式

sodium hydroxide

2,4,5-trifluoroaniline

dimethyl sulfide

N-chlorosuccinimide

→

2-methylthiomethyl-3,4,6-trifluoroaniline

溶媒

dichloromethane

triethylamine

反応条件

後処理

1. 1
   その他is gradually added below 5° C
2. 2
   温度After reflux for 12 hours
3. 3
   抽出extracted with dichloromethane
4. 4
   乾燥the extract is dried over sodium sulfate
5. 5
   濃縮concentrated
6. 6
   その他The residue is purified with column chlomatography (silica-gel, dichloromethane: n-hexane=1:4)

実験手順

To 2,4,5-trifluoroaniline (35.0 g) are added anhydrous dichloromethane (530 ml) and dimethyl sulfide (24.6 ml) and the mixture is cooled to 0° C. Thereto N-chlorosuccinimide (38.2 g) is gradually added below 5° C. After the mixture is stirred at the same temperature for 15 minutes, triethylamine (47.7 ml) is gradually added. After reflux for 12 hours, the resultant is made alkaline with 5% aqueous sodium hydroxide solution, extracted with dichloromethane, and the extract is dried over sodium sulfate and concentrated. The residue is purified with column chlomatography (silica-gel, dichloromethane: n-hexane=1:4) to give 2-methylthiomethyl-3,4,6-trifluoroaniline (22.3 g).

出典