Pressure equalized dropping funnel

A. Methyl 2-oxaayalohexaneaar boxylate. A 500-mL, three-necked, round-bottomed flask is equipped with a mechanical stirrer, reflux condenser, and a pressure-equalizing dropping funnel bearing a nitrogen inlet (Note 1). The flask is flushed with nitrogen and charged with 18.02 g (0.20 mol) of dimethyl... 

A. 2-(Trimethtjlsiloxymethyl)allyltvimethylBilane. An oven-dried (Note 1) 2-L, three-necked, round-bottomed flask is equipped with an air-tight mechanical stirrer (Note 2), a 500-mL pressure-equalizing dropping funnel (Note 3), and a reflux condenser. The top of the condenser is connected to a three-way stopcock with one branch connected to a nitrogen source and the other to a variable pressure oil pump with a dry-ice trap (Note 4). The apparatus is flamed dry under a steady stream of nitrogen. The flask is... 

Methyl-2-propen-l-ol, purchased from Aldrich Chemical Company, was distilled from anhydrous potassium carbonate. It was added directly to the n-butyllithium solution using a long needle. The checkers quickly replaced the pressure-equalizing dropping funnel with a serum cap to carry out this addition. The funnel was fitted to a small dry flask to prevent the introduction of moisture during the addition period and replaced on the reaction flask immediately afterwards. 

A dry 500-ml round-bottomed three-necked flask fitted with a stirrer, internal thermometer, and a pressure-equalized dropping funnel is placed under nitrogen and the flask is charged with 0.148 mole of freshly distilled cyclohexanone and 0.148 mole of freshly distilled ethyl chloroacetate. A solution of 6.0 g of potassium and 125 mL of dry terr-butyl alcohol is introduced into the dropping funnel, and the system is exhausted and... 

N,N Dimethylcyclohexanecarboxamide A 500-ml three-necked flask is equipped with a reflux condenser (drying tube), a pressure-equalizing dropping funnel, and a magnetic stirrer. The flask is charged with 32 g (0.25 mole) of cyclohexanecarboxylic acid and thionyl chloride (45 g, 0.375 mole) is added over 5 minutes to the stirred acid. The flask is heated (oil bath) at a temperature of 150° for 1 hour. The reflux condenser is... 

A 500-ml three-necked flask is fitted with a condenser, a pressure-equalizing dropping funnel, a magnetic stirrer, and a thermometer. The flask is charged with a mixture of 33.6 g (0.48 mole) of 2-methyl-2-butene and 180 ml of a 1 M solution of sodium boro-hydride in diglyme. The flask is cooled in an ice bath and stirring begun. Boron trifluoride etherate (0.24 mole) is added dropwise to the mixture and the solution is stirred at 0° for 2 hours. 

In a 250-ml three-necked flask fitted with a magnetic stirrer, a pressure-equalizing dropping funnel, and a thermometer is placed a solution of l,4-cyclohexanediol(l 1.4g, 0.10 mole), 35 ml of chloroform, and 27 ml of dry pyridine. The solution is cooled in an ice bath to 0-5 and is maintained below 5 throughout the addition. A solution of benzoyl chloride (14 g, 0.10 mole) in 30 ml of dry chloroform is added with stirring at a rate so as to keep the temperature below 5° (approx. 40 minutes). After completion of the addition, the mixture is allowed to come to room temperature and stand overnight. The chloroform solution is washed four times with 50-mI portions of water, once with 50 ml of 5 % sulfuric acid solution, and finally with saturated sodium chloride solution. The chloroform solution is then dried (sodium sulfate), and the solvent is removed. Fractionation of the residue gives a cis and trans mixture of 4-benzoyloxycyclohexanol, bp 175-17870.2 mm, as a very viscous oil, yield about 55%. 

A dry 5(X)-mI flask equipped with a thermometer, pressure-equalizing dropping funnel, and magnetic stirrer is flushed with nitrogen and then maintained under a static pressure of the gas. The flask is charged with 50 ml of tetrahydrofuran and 13.3 ml (0.15 mole) of cyclopentene, and then is cooled in an ice bath. Conversion to tricyclo-pentylborane is achieved by dropwise addition of 25 ml of a 1 M solution of diborane (0.15 mole of hydride see Chapter 4, Section 1 for preparation) in tetrahydrofuran. The solution is stirred for 1 hour at 25° and again cooled in an ice bath, and 25 ml of dry t-butyl alcohol is added, followed by 5.5 ml (0.05 mole) of ethyl bromoacetate. Potassium t-butoxide in /-butyl alcohol (50 ml of a 1 M solution) is added over a period of 10 minutes. There is an immediate precipitation of potassium bromide. The reaction mixture is filtered from the potassium bromide and distilled. Ethyl cyclopentylacetate, bp 101730 mm, 1.4398, is obtained in about 75% yield. Similarly, the reaction can be applied to a variety of olefins including 2-butene, cyclohexene, and norbornene. 

A dry, 500-ml, three-necked flask is fitted with a mechanical stirrer, a condenser, and a pressure-equalizing dropping funnel. The system is swept out with nitrogen and a slight positive pressure of nitrogen is maintained by venting the system to a mercury filled U-tube. In the flask is placed 21 g (0.187 mole) of dry potassium /-butoxide, and the flask is cooled in an ice-salt bath. 

In a 2-1. three-necked flask fitted with an efficient reflux condenser, stirrer, and pressure-equalizing dropping funnel are placed 216 g. (2.0 moles) of anisole (Note 1) and 400 ml. of methylene chloride (Note 2). The reflux condenser is attached to a drying tower. The solution is brought to reflux temperature with a heating mantle, and 167 ml. (278 g., 2.06 moles) of sul-furyl chloride (Note 3) is added dropwise over a 3-hour period. When the addition is complete, heating is continued for an additional 15 hours (Note 4). 

A. Ethyl 4-Amino-3-(methylthiomethyl)benzoate [Benzoic acid, 4-amino-3-[(methylthio)methyl]-]. A 1-1., three-necked, round-bottomed flask is fitted with a mechanical stirrer, a condenser topped with a gas-inlet tube, and a two-neckcd adapter holding a low-temperature thermometer and a 100-ml., pressure-equalizing dropping funnel. The flask is charged with 10.50 g. (0.10 mole) of ethyl p-aminobenzoate [Benzocaine Benzoic acid, 4-amino-, ethyl ester] (Note 1), 300 ml. of acetonitrile, and 100 ml. of dichloromethane, is flushed with nitrogen, and is then immersed in a 40% aqueous methanol-dry ice bath maintained between... 

In a 250-ml., three-necked flask fitted with a mechanical stirrer, a thermometer, and a 25-ml., graduated, pressure-equalizing dropping funnel are placed 7.60 g. (0.050 mole) of phenoxyacetic acid [Acetic acid, phenoxy-] (Note 1), 5.40 g. (0.050 mole) of 1,4-benzoquinone [2,5-Cyclohexadiene-l,4-dioneJ (Note 2), 1 g. (0.006 mole) of silver nitrate [Nitric acid silver(l +) salt] (Note 3), and 125 ml. of water (Note 4). The mixture is then stirred and heated to 60-65° by means of a heating mantle until dissolution is complete. The resulting solution is stirred... 

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