反应详情

温度

0 °C

To a mixed solution of tert-butyl(3S)-4-(1-(diphenylmethyl)azetidin-3-yl)-3-methylpiperazine-1-carboxylate (493 mg, 1.17 mmol) described in Production Example 6-1 and THF (10.0 mL) was added lithium aluminum hydride (178 mg, 4.68 mmol) at 0° C. The resultant mixture was stirred under reflux for 5 hours and 10 minutes. The reaction mixture was cooled to 0° C., then water (178 μL) and a 5 N aqueous sodium hydroxide solution (178 μL) were added thereto, and water (534 μL) was further added thereto. The reaction mixture was filtrated using Celite and then washed with ethyl acetate. A filtrate was concentrated under a reduced pressure, and the resultant residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=2:1) to give the title compound (321 mg, yield: 82%).

1. temperatureunder reflux for 5 hours and 10 minutes
2. filtrationThe reaction mixture was filtrated
3. washwashed with ethyl acetate
4. concentrationA filtrate was concentrated under a reduced pressure
5. customthe resultant residue was purified by NH silica gel column chromatography (heptane:ethyl acetate=2:1)