反应详情

Dissolve 6-[(6-tert-butylthiomethyl-pyridin-3-ylmethyl)-amino]-7-chloro-3-(2,2,2-trifluoroacetyl)-2,3,4,5-tetrahydro-1H-benzo[d]azepine (4.46 g, 9.24 mmol) in methanol (20 mL). Add a solution of potassium carbonate (5.1 g, 37 mmol) in water (10 mL) and stir at room temperature for 12 h. Remove methanol in vacuo, dilute the residue with water, and extract the aqueous phase with DCM. Purify the crude mixture by SCX chromatography (20 g) eluting with methanol and a solution of NH4OH (40 mL) in methanol (140 mL). Concentrate in vacuo to obtain pure 6-[(6-tert-butylthiomethyl-pyridin-3-ylmethyl)-amino]-7-chloro-2,3,4,5-tetrahydro-1H-benzo[d]azepine (3.6 g, 100%). MS (APCI+) m/z: 390 (M+H)+.

1. extractionextract the aqueous phase with DCM
2. customPurify the crude mixture by SCX chromatography (20 g)
3. washeluting with methanol
4. concentrationConcentrate in vacuo