反応 #2186194

反応方程式

chlorocarbonyl-acetic methyl ester

2-Amino-thiophenol

triethylamine

→

desired product

収率 82.0%

Benzothiazol-2-yl-acetic acid methyl ester

収率 82.0%

溶媒

diethylether

diethylether

反応条件

後処理

1. 1
   その他to yield a suspension
2. 2
   その他the precipitate removed by filtration
3. 3
   その他The filtrate is evaporated
4. 4
   その他column chromatographed (silica gel, ethyl acetate/petroleum ether 1:2)

実験手順

3.2 mL (30 mmol) 2-Amino-thiophenol are dissolved in 100 mL diethylether and treated with 4.17 mL (1 eq.) triethylamine to yield a suspension, to which 3.21 mL (1 eq.) chlorocarbonyl-acetic methyl ester in 10 mL diethylether is added dropwise within 20 min. The resulting suspension is stirred and additional 2 h at room temperature, and the precipitate removed by filtration. The filtrate is evaporated and column chromatographed (silica gel, ethyl acetate/petroleum ether 1:2) to yield the desired product as a yellowish liquid (5.1 g, 82%).

出典