反应详情

A stirred mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (10 g, 45.4 mmol), K2CO3 (7.2 g, 52.5 mmol) and N-(2-bromoacetyl)indoline (12 g, 50 mmol) in acetonitrile (300 ml) was heated at reflux for 4 hours. The mixture was cooled and filtered. The solution was concentrated down until solid appeared. The crystals were collected: weight 12.68 g. The mother liquor was concentrated to dryness. The residues were purified further by flash chromatography to yield an additional 1.35 g. Total yield was 14.03 g. A 2 g sample was dissolved in ethanol/methylene chloride and was treated with a solution of fumaric acid (612 mg) in ethanol to yield 2.58 g, m.p. 226°-227° C.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. temperatureThe mixture was cooled
4. filtrationfiltered
5. concentrationThe solution was concentrated down until solid
6. customThe crystals were collected
7. concentrationThe mother liquor was concentrated to dryness
8. customThe residues were purified further by flash chromatography
9. customto yield an additional 1.35 g
10. customto yield 2.58 g, m.p. 226°-227° C.