反应详情

4-(3-Cyclopentyl-2,3,4,5-tetrahydro-1H-benzo[d]azepin-7-yloxy)-piperidine-1-carboxylic acid-tert-butyl ester (E5a) (593 mg, 1.43 mmol) was dissolved in dichloromethane (5 ml) and treated with trifluoroacetic acid (3 ml). The solution was stirred at room temperature for 1 hour, concentrated in vacuo and applied to a SCX ion exchange cartridge (Varian bond-elute, 5 g) and washed with methanol and then a mixture of 0.880 ammonia:methanol (1:9). The combined basic fractions were concentrated in vacuo and the resulting residue was purified by column chromatography eluting with a mixture of 0.880 ammonia:methanol:dichloromethane (1:9:90) to afford the title product (E5). MS (ES+) m/e 315 [M+H]+.

1. concentrationconcentrated in vacuo
2. washwashed with methanol
3. additiona mixture of 0.880 ammonia:methanol (1:9)
4. concentrationThe combined basic fractions were concentrated in vacuo
5. customthe resulting residue was purified by column chromatography
6. washeluting with a mixture of 0.880 ammonia:methanol:dichloromethane (1:9:90)