반응 #640604

반응 방정식

5-acetyl-4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester

hydrochloric acid

→

4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester hydrochloride

용매

EtOH

water

반응 조건

후처리

1. 1
   온도After two hours' heating
2. 2
   온도with refluxing
3. 3
   기타the solution was evaporated
4. 4
   workup.ADDITIONintroduced into 500 mL of cooled EtOAc (ice bath)
5. 5
   기타The resultant precipitate was separated
6. 6
   기타dried under a vacuum

실험 절차

31.1 g (130 mmol) of 5-acetyl-4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester (C) were dissolved in 30 mL of EtOH and combined at RT with 30 mL (260 mmol) of 32% (weight percent) hydrochloric acid solution in water. After two hours' heating with refluxing, the solution was evaporated and introduced into 500 mL of cooled EtOAc (ice bath). The resultant precipitate was separated and dried under a vacuum. 8.13 g (27% of theoretical) of the desired product 4,5,6,7-tetrahydro-isoxazolo[4,5-c]pyridine-3-carboxylic acid ethyl ester hydrochloride (D) were obtained.

출처