Funnel , addition glass

One 50 mL additional funnel with two glass stopcocks, one on a side-arm One filter funnel with glass stopcock on side-arm, diameter 3 cm One lOOmL Schlenk tube Magnetic stirrer plate... 

A. 2-Trimethylsilyloxy-l,3-butadiene (1). An oven-dried 500-ml., three-necked, round-bottomed flask is fitted with two oven-dried addition funnels, a glass stopper, and magnetic stirrer, and placed in a 80-90° oil bath. Under an inert atmosphere, methyl vinyl ketone (25.0 g., 0.357 mole) in 25 ml. of dimethylformamide and chlorotrimethylsilane (43.4 g., 0.400 mole) in 25 ml. of dimethylformamide are added over 30 minutes to a magnetically stirred solution of triethylamine (40.5 g., 0.400 mole) in 200 ml. of dimethylformamide (Note 1). The reaction gradually darkens from colorless to yellow or dark brown, and supports a white precipitate of triethylamine hydrochloride. The reaction is set up to run overnight, or ca. 14 hours. 

Instead of stopping the reaction and opening the apparatus, you can put in the new chemicals using an addition or dropping funnel. Addition funnels are separatory funnels (see p. 119) with a ground-glass joint on the stem, and there are two types (Fig. 16.5) ... 

Another method involves the use of a hopper for the solid (Fig. 5-18) which has a rubber stopper or a glass valve as a seal between the reaction flask and the funnel. Addition is effected by raising the rod attached to the stopper. If the solid clogs the neck of the flask, it may be dislodged by the part of the rod which passes through the stopper. 

A two-necked round flask, addition funnel, magnetic stirrer, septum, syringes. Alter funnel, safety glasses, laboratory coat, and protective gloves. 

A common operation in practical organic chemistry is for stirring, refluxing, and addition of a liquid from a dropping funnel to be carri on simultaneously. The most convenient apparatus for this purpose is a three-necked flask, fitted as in Fig. 11, 7, 11, a. If a three-necked flask is not available, the three-way adapter inserted into a bolt-head flask (Fig. 77, 7, 11, 6) may be used. A further simplification, suitable for elementary students, is to employ a two-way adapter as in Fig. 77, 7, 11, c the stirrer passes through a closely-fitting glass sleeve which is extended... 

If it is desired to carry out the combined operations of stirring, refluxing, and addition of a liquid in a stream of gas, the apparatus of Fig. 77, 7, 12, a may be used the side tube for the gas is sealed on to the separatory funnel. For the passage of a gas into a stirred liquid, the aperture carrying the modified separatory funnel may be fitted with the device shown in Fig. 77, 7, 12, 6 the glass rod inside the tube is held in position by a short length of heavy-wall rubber tubing and is employed to clear the lower end of the gas delivery tube, should it become blocked with solid reaction product. 

Tetrahydrofurfuryl chloride. Place 204 g. (194 ml.) of freshly distilled tetrahydrofurfuryl alcohol (b.p. 177°) and 174 g. (178 ml.) of dry pyridine in a 1-litre three-necked flask, fitted with a dropping funnel, mechanical stirrer and thermometer. Cool in an ice bath, stir vigorously and add 250 g. (153 ml.) of freshly distilled thionyl chloride at the rate of 3-5 drops per second. A pasty crystalline mass begins to separate and the temperar ture commences to rise rapidly when one-third to one-half of the thionyl chloride has been added subsequently the mass largely redissolves and a dark brown liquid forms. Remove the ice bath when the addition is complete and stir the mixture for 3-4 hours. Pour the reaction product into a large separatory funnel and extract with seven 250 ml. portions of ether break up any lumps that may form with a glass rod. Remove the ether from the combined extracts by distillation, wash the residue with three 50 ml. portions of water, dry with anhydrous magnesium sulphate and distil under reduced pressure. The yield of tetrahydrofurfuryl chloride, b.p. 47-48°/15 mm., is 180 g. 

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