Shaker vessels

A high-pressure shaker vessel lined with Hastelloy stainless steel charged with ethylene trithiocarbonate and a little over 2 moles of sulfur tetrafluoride heated 8hrs. at 110° 2,2-difluoro-l,3-dithiolane. Y 82%. F. e. s. R. J. Harder and W. C. Smith, Am. Soc. 83, 3422 (1961). 

The reaction vessels were removed from the reaction module, placed in a shaker rack and treated with 1.00 mL of 9.3 mM HMDS in TFA/CDC13 (1 1). After shaking for 1 h, the contents of the vessels were transferred to 15 mL polypropylene vessels equipped with a filter frit, and the filtrate was collected in 4 mL analytical vials. The cleaved resins were washed three times with... 

FIGURE 5.3 Reaction vessels for solid-phase synthesis. (A) 10-300-mL vessel (0.5-10 g of resin) affixed to a rotating-arc shaker (B) 0.5-8-L (20-200 mm in diameter) cylindrical container with stirrer for up to 500 g of resin (C) Ananth vessel with two 80-mL chambers.10... 

Fmoc-Rink-Nle-pMeBHA-resin (1 g, 0.55 mmol g ) was swollen for 1.5 h in NMP in a reaction vessel equipped with a sintered glass bottom, and placed on a shaker. The Fmoc group was removed with 20% piperidine in NMP (8mL, 2 x 15 min) and after washing with NMP (8mL, 5 x 2 min), the Fmoc removal was monitored by the ninhydrin Kaiser test. Coupling of building blocks such as iV -Fmoc-/Va>-carb-oxyalkyl(OAl)Xaa-OH or /V -Fmoc-/V" -aminoalkyl(Aloc)Xaa-OH, or N -alkylated amino acids such as... 

The enzyme-agarose conjugate, a gel, is stored as a suspension in the immobilization buffer. This gel is rather mechanically fragile. Magnetic stirrers should be avoided, and the contents of reaction vessels gently stirred on a rotary shaker. Attention is drawn to the poisonous nature of cyanogen bromide. 

For each carboxylic acid, TFP resin 34 (20 g with a loading of 1.25 mmol/g) was introduced into a 250-ml glass peptide vessel. The resin was swelled in DMF (120 ml). The carboxylic acid (250 mmol), DMAP (3.05 g, 25 mmol), and DIC (39.14 ml, 250 mmol) were then added sequentially. The reaction was mixed on a wrist shaker overnight. For the workup, the reaction solution was drained and the resin was washed with DMF, THF, DCM, and diethyl ether. The resin was dried in a vacuum oven at room temperature overnight. 

A reaction vessel equipped with a fritted disc, a solvent inlet, and a device to transfer in and out liquids under low nitrogen pressure was used to carry out solid-phase syntheses. This manual apparatus enables suspensions of resin to be stirred either by gently rocking the vessel on a shaker or by bubbling nitrogen through the fritted plate. 

Many kinetic studies investigating reactions on soil constituents have used batch techniques. The traditional batch or tube technique involves placing an adsorbent and the adsorptive in a vessel such as a centrifuge tube. The suspension is stirred or agitated using a reciprocating shaker. Then the suspension is usually centrifuged or filtered to separate a clear supernatant solution for subsequent analysis. 

Shaker table techniques have been developed with increased efficiency for acidic and basic compounds. The sample is placed in an extraction vessel (Erlenmeyer flask or glass jar) together with an extracting solvent, dichloromethane methanol H2SO4 (70 29 1) for acidic compounds or dichloromethane methanol NaOH (70 29 1) for basic compounds. The vessel is placed on a platform shaker for 1 h and then the liquid is decanted into a separatory funnel-containing water. The separatory funnel is gendy shaken, the layers are allowed to separate as for a normal liquid liquid extraction, and the solvent is collected for further processing. 

A Hasteiloy shaker tube (400 mL) was charged with anhyd aluminum chloride fluoride (2 g). cooled to 78 C, evacuated, and charged with hexafluoroacetone (11 49.8 g. 0.3 mol) and trifluorocthcnc (24.6 g, 0.3 mol). The reaction vessel was shaken at 100 C for 18 h. The mixture was bled out of the reactor at 40-50 C and collected in a cold trap( - 78 C). Starting materials were distilled out using a low-temperature distillation column, and the residue was washed with cold HjO and dried (PjO,). It was distilled to give 11 (64% isolated yield, 98% based on converted 13 yield 4 7.6 g) bp 44-45 C. 

To grow the cultures, the inoculated nutrient broths are agitated on a rotary or reciprocal shaker. Shaking prevents sedimentation of solid constituents of the nutrient medium and of the growing culture, and favors homogeneous growth. The vessels arc closed with wadding closures for conventional aerobic transformations, which allows sufficient sterile air to enter the incu-... 

In batch SPPS (solid-phase peptide synthesis), the resin is contained in a vessel, usually equipped for bottom filtration. After a washing solvent or a reagent is added, the resin is mixed and the solvent or reagent is removed by filtration. Batch synthesizers use a variety of methods to mix the resin the wrist-action shaker, vortex mixing, nitrogen bubbling, or overhead stirring. 

In 1989, Advanced ChemTech (ACT) introduced the Model 350 Simultaneous Multiple Peptide Synthesizer capable of assembling up to 96 peptides at scales from 5 to 50 pmol using the Fmoc method. Two different sized reaction vessels are available 600 pL and 1.5 mL. The first Model 350 was originally designed similar to the SMPS 350 by Zinsser, however during the next several years, ACT added additional features, such as an orbital shaker for resin agitation to differentiate the product. ... 

Special reactor bottles having working volumes of 1 mL to 1000 mL are also available. As depicted in Fig. 6.6, these bottles have threaded Teflon adapters to hold the hydrogen inlet tube so catalyst contamination by the reactor is virtually eliminated. The smaller bottles, which have working volumes between 1 mL and 20 mL, use a spacer to secure them into the shaker assembly (Fig. 6.6a). Those with capacities of 20 mL to 200 mL (Fig. 6.6b) fit directly into the shaker assembly of the smaller Parr apparatus while 500 mL and 1000 mL vessels of this type (Fig. 6.6c) are available for the larger unit. 

Aluminum blocks holding (screw-cap) glass reaction vials, which come with either built-in stirring or are mounted on an orbital shaker, are available from STEM, H-i-P, J-Kem or Metz (Table 2, Fig. 4). Reaction vessels normally used are (round-bottomed) glass vials, tubes or bottles. These devices can basically replace a number of magnetic stirplates and, in addition to their making more efficient use of hood space, offer features such as common temperature control. 

Shakers such as the IR-Dancer and CombiDancer (Hettich), the Polyvap (Biichi) or Labconco s RapidVap (Fig. 11) offer the advantage that, in contrast to centrifuges, it is not necessary to balance the mo ving parts. Various sample trays are available, and other vessel formats can be accommodated with custom-made holders. 

As a reaction vessel for resin beads, an array of chromatography tubes or syringes fitted with frits and stoppers can also be used. These can be gently agitated on a shaker ta-... 

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