Funnel , addition

In figure 4 is shown how a separatory funnel and a pressure equalized addition funnel are made. The funnel part is just a PP funnel from the grocery store and what it is attached to is a stainless steel ball valve. See how the addition funnel is made by using a rubber stopper and an extra extension of tubing to the top of the funnel Well, that s how one can make a sealed addition funnel out of the ordinary glass separatory funnel that one gets with a distillation kit or from wherever. 

No matter which flask is used, an addition funnel is required. An addition funnel is just like a separatory funnel except there is an extra side arm that allows for addition into a system that has pressure (which this one is going to have). Strike knows Strike knows Pressure sounds complicated but this one isn t. You ll see. The addition funnel can be bought, made from a separatory funnel as explained in the How to Make section of this book, or... 

The idea is to have everything in place before the oxygen is applied. So, lOOg of safrole is in the addition funnel and stirring around in the reaction flask are 10.6g of PdCU, 60g CuCI and 500mL of aqueous dimethylformamide (made by mixing 62.5mL dH20 and 437,5mL DMF). Dimethylformamide (DMF) is not the same as the watched chemical known as N-methylformamide. 

METHOD 2 [102]-Sodium bicarbonate and dH20 are stirred in a 3-neck flask with two addition funnels attached. One funnel has... 

The intermediates in making amines are isocyanates (0==C==N) just like the Hofmann Rearrangement. The isocyanates are decomposed with water, just like the Hofmann. In fact, there is a lot of similarity between the Hofmann and the Schmidt reactions. Before I detail the synthesis steps, I should note that if you wish to generate the Hydrazoic Acid in the flask by adding Sodium Azide, you might need a powder addition funnel. This bit of equipment is quite pricey and it s likely you won t have one, so the first part of the synthesis details how to make the Hydrazoic Acid separately. 

Prepare a paste out of 65g Sodium Azide (lm NaN ) and 65mL of water in a beaker. Add 400mL of either Chloroform or Benzene to this paste (depending on what you have available, but be consistent later on) and stir well. Dump this mixture into a round bottom flask situated in an ice/salt bath, drop in a stirrer magnet, attach a Claisen adapter, addition funnel, and thermometer. Let this mixture cool to OC. 

Setup your glassware for simple distillation with a claisen adapter, three way adapter, pressure-equalized addition funnel, water cooled condenser, vacuum adapter and receiver flask to catch any condensed solvent vapors. 

The funnel is capped with a rubber septum. For ease of operation, volume markings, corresponding to the amounts of reagents to be added, are put on the addition funnel. 

The checkers used a home-made, glass-jacketed funnel sealed with a rubber septum. The submitters cut one side and part of the bottom of a styrofoam cup and with tape held this in place around the lower part of the addition funnel. 

Tetrahydrofuran, anhydrous, 99.9t (water content <0.006t) was purchased from Aldrich Chemical Company, Inc., and used as received. The vinyl bromide solution was prepared In a 500-mL, round-bottomed flask fitted with a glass stopper. The stoppered flask containing the tetrahydrofuran was chilled to about 5 C and weighed. The vinyl bromide, also chilled to about 5°C, was rapidly poured Into the tetrahydrofuran until the desired amount had been added. The flask was stoppered, the contents mixed by shaking, allowed to warm to about 16°C, and then added to the pressure-equalizing addition funnel. 

Cyalohexylideneaaetonit ri-le. A 1-L three-necked, round-bottomed flask equipped with a reflux condenser, mechanical stirrer and addition funnel, is charged with potassium hydroxide (855 pellets, 33.0 g, 0.5 mol. Note 1) and acetonitrile (250 ml. Notes 2 and 3). The mixture is brought to reflux and a solution of cyclohexanone (49 g, 0.5 mol. Note 4) in acetonitrile (100 mL) is added over a period of 0.5-1.0 hr. Heating at reflux is continued for 2 hr (Note 5) after the addition is complete and the hot solution is then poured onto cracked ice (600 gl. The resulting binary mixture is separated... 

Any crystals which may form at the tip of the addition funnel are scraped off and allowed to drop into the reaction flask. 

B. cis-1,2-Gyclohexanedimethanol Dimethanesulfonate. In a 5-1., three-necked, round-bottomed flask, immersed in an ice-salt bath and fitted with a mechanical stirrer and an addition funnel, is plaeed a solution of 111 g. (0.97 mole) of methanesulfonyl chloride in 1.21. of pyridine. While cooling and stirring, a solution of 46.4 g. (0.322 mole) of m-l,2-cyclohexanedimethanol in 250 ml. of pyridine is added dropwise at a rate such that the temperature does not exceed 0° (Note 5). Upon completion of the addition, the mixture is stirred at — 5° to 0° for an additional 2 hours. Two liters of cold 10% hydrochloric acid is introduced at a rate which maintains the reaction mixture below 20° (Note 5). The solid which separates is isolated by suction filtration, washed sequentially with 11. of dilute hydrochloric acid and 21. of water, and air-dried. There is isolated 93-95 g. (96-98%) of the dimethanesulfonate having m.p. 66-67.5°. Reorystallization from methanol gives needles melting at 75-76° (Note 6). 

B. Tropohne. In a 1-1., three-necked, round-bottomed flask equipped with a mechanical stirrer, addition funnel, and reflux condenser are placed 500 ml. of glacial acetic acid and then, cautiously, 100 g. of sodium hydroxide pellets. After the pellets have dissolved, 100 g. of 7,7-dichlorobicyclo[3.2.0]hept-2-en-6-one is added and the solution is maintained at reflux under nitrogen for 8 hours. Concentrated hydrochloric acid is then added until the mixture is about pH 1 approximately 125 ml. of acid is required. After the addition of 1 1. of benzene, the mixture is filtered and the solid sodium chloride is washed with three 100-ml. portions of benzene. The two phases of the filtrate are separated and the aqueous phase is transferred to a 1-1. continuous extractor (Note 8) which is stirred magnetically. The combined benzene phase is transferred to a 2-1. pot connected to the extractor and the aqueous phase is extracted for 13 hours. Following distillation of the benzene, the remaining orange liquid is distilled under reduced pressure... 

B. Methylenecyclohexane. A 500-ml. three-necked round-bottomed flask is fitted with a reflux condenser, an addition funnel, a mechanical stirrer, and a gas inlet tube. A gentle flow of nitrogen through the apparatus is maintained throughout the reaction. An ethereal solution of -butyllithium (0.10 mole, about 100 ml., depending on the concentration of the solution) and 200 ml. of anhydrous ether is added to the flask. The solution is stirred and 35.7 g. (0.10 mole) of triphenylmethylphosphonium bromide is added cautiously over a 5-minute period (Note 2). The solution is stirred for 4 hours at room temperature (Note 3). 

The dry tosylhydrazone (20 g, 45.5 mmol) is dissolved in 750 ml of 1,2-dimethoxyethane (freshly distilled from lithium aluminum hydride) in a flame-dried 1 liter round bottom flask fitted with a 240 ml addition funnel, a drierite tube and a magnetic stirrer. A 2.05 M ether solution of methyllithium (130 ml, Alfa Inorganics, Inc.—Caution to avoid the mineral oil impurity the methyllithium solution is decanted from a cold solution which contains a precipitate) is placed in the dropping funnel and added over a 60 min period. The temperature of the reaction mixture increases to ca. 35° during the addition however, no cooling precautions are required. The highly colored reaction mixture is stirred for 7 hr and then poured into 1.5 liters of ice water. The flocculent precipitate is digested for 12 hr at room temperature to speed the filtration. After filtration the filter cake is washed with 500 ml water and dried under vacuum at 50° for several hr. The androsta-5,16-dien-3l5-ol is obtained in ca. 70% yield after recrystallization from methanol mp 138-139°. 

In a three-necked flask fitted with a thermometer, a stirrer, a condenser (drying tube), and a pressure-equalizing addition funnel, HMPT (25 ml, 0.14 mole) and anhydrous ether (30 ml) are introduced. Finely divided lithium (1.75 g, 0.25 g-atom) is then added... 

A 500-ml, three-necked, round-bottom flask is fitted with a mechanical stirrer, a pressure-equalizing addition funnel and a reflux condenser (drying tube). The flask is charged with 100 ml of dry dimethylformamide, 9.2 ml (0.1 mole) of dry -butyl alcohol, and 28 g (0.107 mole) of dry triphenylphosphine. The flask is cooled in a water bath, stirring is begun, and bromine (approx. 16 g, 0.1 mole) is added over about 15 minutes. 

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