반응 #2879
ord-6f47bc261884491694bca9fab87d052d
반응 방정식
반응물
시약
반응 조건
후처리
- 1온도the mixture was cooled to about 55° C.
- 2온도The resulting mixture was heated to 80° C
- 3기타was consumed
- 4기타Upon complete reaction
- 5온도to cool to room temperature
- 6농축the organic layer concentrated in vacuo at 40° C.
- 7기타The resulting oil was used in the next step without further purification
실험 절차
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.