反应 #2879
ord-6f47bc261884491694bca9fab87d052d
反应方程式
反应物
试剂
反应条件
后处理
- 1温度the mixture was cooled to about 55° C.
- 2温度The resulting mixture was heated to 80° C
- 3其他was consumed
- 4其他Upon complete reaction
- 5温度to cool to room temperature
- 6浓缩the organic layer concentrated in vacuo at 40° C.
- 7其他The resulting oil was used in the next step without further purification
实验过程
A mixture of ethyl 4-hydroxybenzoate (8.31 g), 1-(2-chloroethyl)piperidine monohydrochloride (10.13 g), potassium carbonate (16.59 g), and methyl ethyl ketone (60 mL) was heated to 80° C. After one hour, the mixture was cooled to about 55° C. and treated with additional 1-(2-chloroethyl)piperidine mono-hydrochloride (0.92 g). The resulting mixture was heated to 80° C. The reaction was monitored by thin layer chromatography (TLC), using silica-gel plates and ethyl acetate/acetonitrile/triethylamine (10:6:1, v/v). Additional portions of 1-(2-chloroethyl)piperidine hydrochloride were added until the starting 4-hydroxybenzoate ester was consumed. Upon complete reaction, the reaction mixture was treated with water (60 mL) and allowed to cool to room temperature. The aqueous layer was discarded and the organic layer concentrated in vacuo at 40° C. and 40 mm Hg. The resulting oil was used in the next step without further purification.