Water → 4-(4-Methoxy-5-isoquinolyl)amino-1-(tert-butoxycarbonyl)piperidine

温度

65 °C

A suspension of Intermediate 71 (600 mg) and copper(I) iodide (141 mg, Kanto Chemicals) in methanol (5.5 ml) and pyridine (5.5 ml) was added with sodium methoxide (28% methanol solution, 1.7 ml, Wako Pure Chemical Industries) and stirred with heating at 65° C. for 24 hours. The reaction mixture was cooled to room temperature, then added with water (30 ml) and extracted three times with ethyl acetate (20 ml for each time). The combined organic layer was washed twice with saturated brine (30 ml for each time) and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2) to obtain the title compound (364 mg).

1. temperatureThe reaction mixture was cooled to room temperature
2. extractionextracted three times with ethyl acetate (20 ml for each time)
3. washThe combined organic layer was washed twice with saturated brine (30 ml for each time) and
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=1:2)

ORDレコード

ord-e66b85a64f8c49938e94e99c298be080

出典データセット

uspto-grants-2006_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07094789B2