Water → HCID 86584271, compound

Participants

Reaction Steps

The dibutyltin intermediate was prepared by a synthetic procedure reported in the literature. The diol 4 (80.4 g, 0.61 moles) was dissolved in 1 L toluene and transferred to a three-neck, 2-L flask fitted with a mechanical stirrer, thermometer, Dean Stark trap with extension adapter, and a reflux condenser. To the stirred reaction mixture was added 153.8 g 98% purity di-n-butyltin oxide, (Bu)2SnO. The mixture was then heated to reflux to azeotrope off the water of reaction. Initially, considerable foaming resulted and care was taken to prevent overflow into the Stark trap. The last traces of H2O were slowly removed at reflux (4 to 5 hr); total H2O collected: ˜11 mL. The mixture (a deep orange-brown color) was cooled to room temperature.

Provenance & Evidence