反应 #1178487

反应方程式

Bis-(2-oxoethyl)carbamic acid benzyl ester

1,1-dimethyl-2-fluoroethylamine hydrochloride

dichloroethane

sodium triacetoxyborohydride

→

title compound

收率 40.0%

4-(1,1-Dimethyl-2-fluoroethyl)piperazine-1-carboxylic acid benzyl ester

收率 40.0%

溶剂

sodium hydrogen carbonate

反应条件

后处理

1. 1
   workup.ADDITIONwas added
2. 2
   workup.STIRRINGthe mixture was stirred for 30 minutes
3. 3
   萃取extracted with methylenechloride
4. 4
   洗涤The extract was washed with saturated brine
5. 5
   干燥dried over anhydrous sodium sulfate
6. 6
   浓缩the solvent was concentrated under reduced pressure
7. 7
   其他The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 40S, n-hexane/ethyl acetate=1/1 to ethyl acetate)

实验过程

Bis-(2-oxoethyl)carbamic acid benzyl ester (0.81 g, 3.45 mmol) and 1,1-dimethyl-2-fluoroethylamine hydrochloride (0.40 g, 3.14 mmol) were dissolved dichloroethane (50 mL), and sodium triacetoxyborohydride (1.99 g, 9.41 mmol) was added thereto. The mixture was stirred for three days at room temperature. A saturated aqueous solution of sodium hydrogen carbonate (20 mL) was added to the reaction liquor, and the mixture was stirred for 30 minutes, and then extracted with methylenechloride. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and then the solvent was concentrated under reduced pressure. The obtained residue was purified by flash chromatography (Flash Chromatography System from Biotage AB, column size: 40S, n-hexane/ethyl acetate=1/1 to ethyl acetate), to obtain the title compound (370 mg, 29%), partially including impurities, as an oily matter.

来源