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6.5 g. (0.030 mole) of ethyl 2-methyl-4-piperidinobutyrate was combined with a mixture of 45 ml. of water and 45 ml. of concentrated hydrochloric acid and heated at reflux for 16 hours. The solution was concentrated under reduced pressure (water aspirator) to give a residue which crystallized upon addition of 50 ml. of diethyl ether. The ether was decanted, and the solid was triturated with acetone and filtered. Recrystallization from acetic acid/acetone gave 3.38 g. of colorless crystals, m.p. 166°-168°C. and a second crop of 1.27 g. of solid, m.p. 165°-168°C. The total yield for both batches was 69%. Anal. Calcd. for C10H20ClNO2 (MW = 221.72): C, 54.20; H, 9.09; N, 6.32; Found: C, 54.17; H, 9.15; N, 6.36.

1. temperatureat reflux for 16 hours
2. concentrationThe solution was concentrated under reduced pressure (water aspirator)
3. customto give a residue which
4. customcrystallized upon addition of 50 ml
5. customThe ether was decanted
6. customthe solid was triturated with acetone
7. filtrationfiltered
8. customRecrystallization from acetic acid/acetone
9. customgave 3.38 g
10. customThe total yield for both batches