反应详情

温度

0 °C

The above oil 3(R)-[(2S,5R)-2,5-dihydro-3,6-dimethoxy-5-(1-methylethyl)-2-pyrazinyl]-3-(4-methoxyphenyl)propanol (28) (17.7 g) was dissolved in 300 mL of dichloromethane. To the solution at −5° C. was added methane sulfonyl chloride (8.02 g, 5.42 mL, 70 mmol) followed by diisopropylethylamine (DIPEA, 12 mL, 70 mmol) dropwise over 10 min. The reaction was stirred at 0° C. for 2 hour. The light yellow solution was diluted with 2 L of ether and was washed with water (3×200 mL) and brine (2×200 mL). After it was dried over sodium sulfate, the solution was concentrated to a volume of 160 mL under vacuum at 20° C. TLC in EA/H (=1:1): Rf=0.74, as a major spot; Rf=0.21, as a minor spot.

1. washwas washed with water (3×200 mL) and brine (2×200 mL)
2. dry with materialAfter it was dried over sodium sulfate
3. concentrationthe solution was concentrated to a volume of 160 mL under vacuum at 20° C