反应详情

温度

70 °C

Thionyl chloride (0.139 ml, 1.90 mmol) was added dropwise to a solution of 12-2 (200 mg, 1.27 mmol) in MeOH (2 ml) at room temperature. After addition was complete, the reaction was heated in a sealed vessel at 70° C. for 2 h. The reaction was cooled to room temperature and concentrated in vacuo. The residue was diluted with 7N NH3/MeOH (3 mL) and filtered to remove insolubles. The filtrate was concentrated to dryness to afford 12-3 as a clear oil.

1. additionAfter addition
2. temperatureThe reaction was cooled to room temperature
3. concentrationconcentrated in vacuo
4. additionThe residue was diluted with 7N NH3/MeOH (3 mL)
5. filtrationfiltered
6. customto remove insolubles
7. concentrationThe filtrate was concentrated to dryness