Fischer Porter tube

A soln. of 1,2-dimethyl-1,4-cyclohexadiene in 3.6 10 water/acetone added to a yellow slurry of bis(acetonitrile)dichloropalladium(II), KHCO3, and CUCI2 in acetone at 20°, and worked up after 24 h di-p-chlorobis[(l,2,3-r )-5-hydroxy-l,2-dimethyl-2-cyclohexen-l-yl]dipalladium (Y 77%), in methanol containing Na-propionate pressurized in a Fischer-Porter tube with 3.8 atm. CO for 4.5 h methyl trans-S hydroxy-... 

A 90 mL Fischer-Porter tube was charged under nitrogen with the catalyst 2 (0.02 mmol), an ester (2 mmol) and 1,4-dioxane (2 mL) followed by filled with H2 (5.3 atm). The solution was heated at 115°C (actual solution temperature) with stirring for the specified period. After cooling to room temperature, excess H2 was vented carefully and the product yields were determined by GC. 

Catalyst (0.2-1 mol%), di-esters, H2 and dry THF (3-5 mL) were heated in a Fischer-Porter tube or a high-pressure reactor at 110°C (oil bath temperature) and the yields of 1,2-diols were analysed by GC. In the case of complex 9a, 1 equiv. (relative to Ru) of KO Bu was used for the in-situ generation of the dearomatized catalyst. 

Catalyst, methyl formate, H2 and dry THF (3-5 mL) were heated in a Fischer-Porter tube or a high-pressure reactor at specified temperature and the yields of methanol were quantified on GC. 

It is noteworthy that further reaction of species (32) in acetone with 5 atm of H 2 gas in a Fischer Porter tube at 65 °C affords the novel trimeric cduster complex (34) (Scheme 2.18). In this compound, the Pt atoms are connected by metal-metal bonds and by three bridging carbonyl ligands, forming a rigid cluster (Scheme 2.18). 

Pcntacarbonyl[(methoxy)(methyl)carbene]chromium(0) (16, R1 = R2 = Me 475 mg, 1.9 mmol) and the chiral ene carbamate (see above equation) (718 mg, 3.8 mmol) in CH2Ci2 (20 mL) were placed in a Fischer Porter pressure tube and saturated with CO (3 eycles to 6.33 atm of CO) and then irradiated (450-W Conrad-Hanovia 7825 medium-pressure lamp, Pyrex well) under 6.33 atm CO overnight. The yellow-green solution was filtered through a pad of Cclitc, and the solvent evaporated. The crude mixture was placed in a sublimation apparatus and heated at 30-50°C (1 Torr) until no further Cr(CO)6 could be obtained. The residue was preabsorbed on silica gel and flash chromatographed yield 319 mg (61 %) mp 133-134"C. 

In a dry-box operation, a 3-ounce Fischer-Porter aerosol compatibility tube is loaded with approximately 10 g. of cesium fluoride and then equipped with a stainless-steel needle-valve adapter and a 323A Hoke valve, f After removal from the dry-box, Swagelokf connections are made from the valve to a metal standard-taper joint and the whole assembly attached to... 

To 5 gm vinylferrocene in 5 ml benzene in Fischer-Porter aerosol compatibility tubes equipped with valves is added 2.52 wt% of azobisisobutyronitrile, based on vinylferrocene. Caution benzene is extremely toxic.) The tubes are degassed by three alternate freeze-thaw cycles and then filled with nitrogen to slightly above ambient pressure and placed in a 80°C constant-temperature bath. After 2 hr, another portion (2.48 wt%) of azobisisobutyronitrile is added and the heating continued for a total of 20 hr. The tube is cooled, vented, and the polymer is precipitated in methanol. The polymer is purified by two more precipitations and then dried at 70°-80°C under vacuum to give 3.1 gm (62.4% yield), m.p. 281°-285°C (yellow powder). 

Conditions Complex 16 (0.01 mmol), alcohol (10 mmol), ammonia (7.5 atm), and toluene (3 ml) were heated in a Fischer-Porter glass pressure tube... 

Irradiation Procedure. Reaction mixtures were prepared at room temperature by transferring desired quantities of reactants from their storage bulbs to the reaction vessel, a 500-cc. spherical borosilicate glass flask attached to the vacuum line by a section of glass capillary tubing and a 4-mm. bore threaded glass valve with a Teflon plug (Fischer and Porter 795-609). Prior to each experiment this vessel was baked under vacuum at 500°C. for 12 or more hours. 

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