Organic 2 Review Problem 273

Organic 2 Review Problem 273 - P REPARATIONS 257 bath in a...

Info iconThis preview shows page 1. Sign up to view the full content.

View Full Document Right Arrow Icon
PREPARATIONS 257 bath in a fume-cupboard and add slowly down the condenser, from a calibrated dropping-tube, 2 ml. of acetyl chloride. Shake the flask after each addition (about 0-5 ml. at a time). When all the acetyl chloride has been added, fit the top of the condenser with a calcium chloride tube bent downwards (cf. Fig. 61, p. 105), and heat the flask in the water-bath at 50° for about 30 minutes. This usually suffices to remove all the hydrogen chloride. When no more hydrogen chloride is evolved pour the mixture into a ioo ml. flask containing 20 ml. of water. Shake the flask vigorously: aluminium chloride and hydrogen chloride are thus extracted by the water. Now pour the mixture into a small separating-funnel and run off the lower aqueous layer. Wash the benzene layer with dil. NaOH solution and again run off the lower layer. Transfer the benzene layer to a small dry flask and dry with anhydrous calcium chloride for 15 minutes. Transfer the dry benzene solution (or a portion of it at a time) to a 10 ml. pear-shaped flask
Background image of page 1
This is the end of the preview. Sign up to access the rest of the document.
Ask a homework question - tutors are online