反应详情

温度

-40 °C

1.3 g of 4-(3,6-dihydro-2H-pyran-4-yl)morpholine were dissolved under argon in 12 ml of THF, the mixture was cooled to −40° C., and then 1.3 g of sulfamoyl chloride were added, followed by 6 ml of diisopropylamine. The cooling was removed and, after the mixture had come to room temperature, it was stirred for another 2 hours. An oil separated out. The THF was decanted off, and the residue was taken up in methanol and filtered through silica gel. The filtrate was concentrated under reduced pressure and the residue, bound to 12 g of Celite, was purified by means of a silica gel column (50 g): solvent A: dichloromethane, B: methanol, gradient: 0 min 2% B, 3 min 2% B, 5 min 5% B, 35 min 10% B, 45 min 10% B; flow rate 20 ml/min; detection: 220 nm, fraction size: 20 ml. After removal of the solvent under reduced pressure, the product was thus obtained with impurities. The residue (1.09 g) was used further without further workup.

1. customThe cooling was removed
2. customhad come to room temperature
3. customAn oil separated out
4. customThe THF was decanted off
5. filtrationfiltered through silica gel
6. concentrationThe filtrate was concentrated under reduced pressure
7. customwas purified by means of a silica gel column (50 g)
8. custom0 min 2% B, 3 min 2% B, 5 min 5% B, 35 min 10% B, 45 min 10% B
9. customAfter removal of the solvent under reduced pressure
10. customthe product was thus obtained with impurities