反応 #81610

反応方程式

4-chlorobenzenesulphonyl chloride

ethyl 3-(2-aminoethyl)-5-[(4-fluorophenyl)methyl]benzenepropanoate

triethylamine

→

title compound

収率 73.2%

Ethyl 3-[2-[(4-chlorophenyl)sulphonylamino]ethyl],5-(4-fluorophenylmethyl)benzenepropanoate

収率 73.2%

溶媒

dichloromethane

反応条件

後処理

1. 1
   洗浄washed with water
2. 2
   乾燥dried (MgSO4)
3. 3
   その他The solvent was evaporated
4. 4
   その他the residue was chromatographed on silica gel
5. 5
   洗浄Elution with dichloromethane first gave impurity
6. 6
   その他evaporated

実験手順

4-chlorobenzenesulphonyl chloride (352 mg) was added portionwise to a stirred solution of ethyl 3-(2-aminoethyl)-5-[(4-fluorophenyl)methyl]benzenepropanoate (500 mg) and triethylamine (0.25 ml) in dry dichloromethane (5 ml) at room temperature. The solution was stirred at room temperature for 5 hours and then washed with water and dried (MgSO4). The solvent was evaporated and the residue was chromatographed on silica gel. Elution with dichloromethane first gave impurity followed by pure product. The product fractions were combined and evaporated to give the title compound as an oil (560 mg); Rf 0.2 (SS 3). Found: C,62.08; H,5.47; N,2.73. C26H27ClFNO4S requires C,61.96; H,5.40; N,2.78%.

出典