反应详情

A mixture of 1-(6-amino-5-chloro-2-methoxy-3-pyridinyl)-3-(1-isobutyl-4-piperidinyl)-1-propanone (step 1 in example 15, 50 mg, 0.141 mmol) in 10% methanolic hydrochloric acid (1 ml) was refluxed for 4 h. To this mixture, concentrated hydrochloric acid (0.2 ml) was added and the mixture was refluxed for 4 h. After cooling to room temperature, the mixture was concentrated in vacuo, treated with SCX column gave brown oil. This oil was chromatographed on a column of silica gel eluting with 25% ammonium hydroxide/methanol/dichloromethane (0.1:1:10) to give pale yellow solid, which was washed with ethyl acetate to afford 19.5 mg (40%) of the title compound as pale orange solids.

1. temperaturewas refluxed for 4 h
2. temperaturethe mixture was refluxed for 4 h
3. concentrationthe mixture was concentrated in vacuo
4. additiontreated with SCX column
5. customgave brown oil
6. customThis oil was chromatographed on a column of silica gel eluting with 25% ammonium hydroxide/methanol/dichloromethane (0.1:1:10)
7. customto give pale yellow solid, which
8. washwas washed with ethyl acetate