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温度

0 °C

To a mixture of 146a (1.50 g, 6.55 mmol) in CHCl3 (60 mL) cooled at 0° C. was slowly added SOCl2 (2.34 g, 19.6 mmol) while maintaining the internal temperature below 5° C. This reaction mixture was warmed to 50° C. and stirred at this temperature for 3 h. It was then cooled to 0° C. and quenched with water. The organic layer was separated and evaporated under reduced pressure. The residue was purified by silica-gel column chromatography eluting with 30:1 dichloromethane/methanol to afford 146b (1.1 g, 68%) as a yellow solid. MS-ESI: [M+H]+ 247.9

1. temperaturewhile maintaining the internal temperature below 5° C
2. temperatureThis reaction mixture was warmed to 50° C.
3. temperatureIt was then cooled to 0° C.
4. customquenched with water
5. customThe organic layer was separated
6. customevaporated under reduced pressure
7. customThe residue was purified by silica-gel column chromatography
8. washeluting with 30:1 dichloromethane/methanol