反应详情

温度

10 °C

Stir a solution of N-((1R,3S)-5-isopropoxy-6-methyl-3-(4-piperidinyl)-1-isochromanyl-methyl)formamide (200 mg, 0.58 mmole) in dichloromethane (3 mL), cool to 10° C. and add 2-phenylbutyryl chloride (115 mg, 0.64 mmole) and triethylamine (88 mg, 0.87 mmole). Allow to warm to room temperature and pour into dilute HCl. Separate the layers an extract the aqueous layer two times with 4 mL of dichloromethane. Wash the combined organic extracts with water and dry over Na2SO4. Purify the crude product on a 10 g silica gel column (eluting with ethyl acetate:heptane 3:1). Collect the appropriate fractions and concentrate to obtain the title compound. It was used without further purification in the next step.

1. temperatureAllow to warm to room temperature
2. customSeparate the layers
3. extractionan extract the aqueous layer two times with 4 mL of dichloromethane
4. washWash the combined organic extracts with water
5. dry with materialdry over Na2SO4
6. customPurify the crude product
7. washon a 10 g silica gel column (eluting with ethyl acetate:heptane 3:1)
8. customCollect the appropriate fractions
9. concentrationconcentrate