Adapter, Claisen inlet

B. (3-Bromo-3,3-difluoropropyl)trimethylsilane. A 1-L, four-necked flask is equipped with a mechanical stirrer, thermometer, Claisen adapter, septum inlet, reflux condenser (the top of which is connected to a calcium chloride drying tube), and a solid addition funnel. The flask is charged with (1,3-dibromo-3,3-difluoropropyl)trimethylsilane (78.3 g, 0.25 mol), and anhydrous dimethyl sulfoxide (200 mL), and the solid addition funnel is charged with sodium borohydride (11.5 g, 0.30 mol) (Notes 7 and 8). The stirred solution is warmed to 80°C, and sodium borohydride is added at a rate sufficient to maintain a reaction temperature of 80-90°C (Note 9). Toward the end of the addition, an additional portion of dimethyl sulfoxide (200 mL) is added via syringe to lower the viscosity of the reaction mixture. After the addition is complete, the mixture is cooled in an ice-water bath, diluted with 100 mL of pentane, and cautiously quenched with 12 M hydrochloric acid until no further gas evolution occurs. The mixture is transferred to a separatory funnel and washed with three, 100-mL portions of 5% brine. The pentane extract is dried over calcium chloride and the solvent removed through a 15-cm Vigreux column. Further fractionation yields 41.5 g (72%) of 3-bromo-3,3-difluoropropyltrimethylsilane, bp 139-141 °C (Note 10). 

A 100-ml. Claisen distillation flask with two 14/20 standard taper joints and a thermometer inlet is equipped with a gas inlet adapter, a... 

A Claisen adapter can be added to allow use of both inlet tube and thermometer. If you must decide between the two then pick the inlet tube. 

A 500-mL, three-necked, round-bottomed flask is equipped with a 25-mL pressure-equalizing dropping funnel, a mechanical stirrer, and a Claisen adapter fitted with a nitrogen inlet adapter and a low temperature thermometer (Note 1). The flask is charged with 11.5 g (0.077 mol) of (R)-(-)-carvone (Note 2), 10.8 g (0.079 mol) of 1-methyl-l-(trimethylsilyl )allene (Note 3), and 180 mL of dry dichloromethane (Note 4), and then cooled below -75°C with a dry ice-acetone bath while a solution of 17.4 g (0.092 mol) of titanium tetrachloride (Note 5) in 10 ml of dichloromethane is added dropwise over 1 hr. After 30 min, the cold bath is removed, and the reaction mixture, which appears as a red suspension, is allowed to warm to 0°C over approximately 30 min. The resulting dark red solution is poured slowly into a 2-L Erlenmeyer flask containing a magnetically-stirred mixture of 400 mL of diethyl ether and 400 mL of water (Note 6). The aqueous phase is separated and extracted with... 

In a hood, set up a 1-liter four-necked flask fitted with a mechanical stirrer, two Claisen-type adapters to accommodate a reflux condenser, a 250-ml addition funnel, a nitrogen inlet tube, a thermometer, and a 50-ml addition funnel. 

A. Methyl 3.6-dimethyl-3-hydroxy-6-heptenoate (Note 1). An oven-dried, threenecked, 500-mL, round-bottomed flask, is fitted with an efficient mechanical stirrer, a Claisen adapter bearing a reflux condenser with a nitrogen, inlet and rubber septum, and a thermometer. The flask is maintained under a static nitrogen pressure and charged with 5-methyl-5-hexen-2-one (24.20 g, 0.216 mol) (Note 2), trimethyl borate... 

Bromo(ethoxycarbonyl)fluoromethyl]phenylmercury A 500-mL, three-neck flask equipped with an addition funnel, paddle stirrer, and Claisen adapter with low-temperature thermometer and an Nj inlet was charged with chlorophenylmercury (9.39 g, 30 mmol), ethyl bromofluoroacetate (6.61 g, 35.6 mmol), and THF (100 mL). In the addition funnel was prepared a solution of r-BuOK (3.93 g, 35 mmol) in THF (50 mL), precipitated as the alkoxide by addition of r-BuOH (33 mL, ca. 35 mmol). 

The glassware is assembled hot under nitrogen as for the previous step. The nitrogen inlet and stirrer are mounted on a Claisen adapter, and the thermometer is removed during the flushing period, then reinserted. 

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