472 g of 2-methyl-2,4-pentanediol (4 moles) are heated to 70°-80°C in a
bowl, and 660 g of chloral hydrate (4 moles) are added under stirring until all
of chloral hydrate is dissolved. The temperature, which decreases during the
addition, then increased to 60° to 70°C. When reaction mixture has become a
nearly dry crystal powder, the powder is subjected to further drying by slight
heating. Yield of raw product is about 1060 g. Recrystallization is carried out
from tetrachloromethane, and the yield is 980 g (about 92 %).