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6.2.5 Special Applications 6.2.5.1 Process Development

Process development is a multiparameter optimization problem. It is not surprising, therefore, that now that the technology is available to parallelize and automate organic synthesis, it is applied in this field.

Three systems designed for solution-phase synthesis and especially process development are currently available: Anachem SK233, Argonaut Surveyor and BOHDAN (Table 7). The latter two are especially designed for the process chemist who wishes to evaluate different reaction conditions such as temperatures, solvents, etc. The BOHDAN instrument offers the possibility to set the temperature individually for each reaction vessel.

Table 7. Equipment for parallel process development

Argonaut Surveyor

Bohdan Process optimization workstation

Gilson Anachem SK 233

Reaction vessels

Material/shape

Number/volume

Reagent vials Number/volume online solvents Agitation

Temperature range

Inert atmosphere Reflux capability waste segregation On line sampling Fully enclosed

Teflon vessels up to 10/75 ml (wv 15-45 ml)

up to 28/40 ml + bulk reagents min. 4

vertically moving magnetic bar

glass tubes up to 12/20 ml wv

• common reagents 2/125 ml, stirred (-10°C to 50 °C)

• slurry 2/125 ml, stirred glass tubes up to 20/ca. 10 ml wv up to 28/40 ml magnetic stirring

-20 to 140°C (temperature can be set individually for each vessel)

3/250 ml each magnetic stirring

6.2.5.2 Equipment for Parallel Reactive Gas Chemistry

Zinsser SOPHAS, Argonaut Quest, ACT Vantage/Venture, Chemspeed as well as the Calypso reaction blocks already possess (limited) reactive gas chemistry capabilities. Recently, instruments dedicated to perform pressurized gaseous reactions have appeared: Bohdan developed a high-pressure synthesizer which is capable of running 12 reactions (30 ml total volume each) simultaneously at pressures up to 13 atm (200 psi). Argonaut Technologies have devised a high-pressure synthesizer named "Endeavor". This machine allows up to eight reactions to be performed at pressures up to 500 psi and temperatures up to 200° C.The reaction vessel working volume is 5 ml (total volume 15 ml). Gas uptake and pressure changes over time can be monitored.

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