1 liter of distilled water in a 2 liter beaker with vigorous stirring a milky emulsion formed but soon solid began to deposit on the walls of the beaker and the liquid slowly cleared after stirring for another 30 minutes the crystalline solid was scraped off and the suspension of liquid and crystals filtered on a 7 cm buchner funnel using a 4 filter paper the off white solid was washed repeatedly with water and sucked dry on the filter the damp dried product weighed 37 g and after drying at 45 u00b0 c in a vacuum oven weighed 32 5 g 88 theory the crude product was recrystallized from 160 ml methanol and gave a white crystalline solid weighing 24 6 g 66 theory mp 68 70 u00b0 c a second recrystallization raised this to 69 70 u00b0 c identical with the material prepared from the tosylate to a labcrest pressure bottle containing 200 ml methanol and 0 94 g of pre reduced 10 pd carbon catalyst was added 18 5 g 0 05 mol of 5 4 carbomethoxyphenoxy 2 benzyloxy isoidide after several cycles of 75 psi n 2 followed by evacuation to lt 0 5 mm hg the manifold was pressurized to 75 psi with hydrogen and stirring was begun over a period of 18 hrs.