In a beaker 33 g of chloral hydrate is dissolved in 40 mL of water with vigorous stirring then a solution is prepared from very cold water, 0.5 g of sodium hydroxide and 3 g of sodium borohydride, the chloral hydrate beaker is immersed in an ice water bath and slow addition of the borohydride is started. The temperature should be maintained below 30°C, after the addition, the solution is stirred for 15 minutes and then 5% HCl is added until no bubbling occurs. The product is extracted from the solution twice with 50 mL of DCM, the solution is then distilled and a fraction of 151-152°C is collected.
Addition of the borohydride solution
Stirring for further 15 minutes
Extraction of the product with DCM