ABSTRACT
Key features of a well-documented experimental procedure include:
1.statement of grams and moles of all reactants used;
2.statement of grams and moles of all catalysts and ligands used;
3.statement of volumes of all reaction solvents used;
4.statement of reaction temperature, reaction pressure (if different from 1 atm), and reaction time;
5.for the work-up procedure, statement of the volumes of all aqueous and organic extraction solvents, and masses of decolorizing charcoal, filtering agents, and drying agents;
6.for the purification procedure, statement of the volumes of recrystallization solvents and chromatographic solvents, and mass of silica gel or alumina packing material;
7.documentation of any color changes, gas evolution, precipitation, or heat evolution that may occur during the course of the reaction;
8.documentation of all cautionary and safety notes in carrying out the reaction;
9.statement of the size of the reaction vessel and the number of ports (necks);
10.statement of any specialized glassware that is required (e.g., dropping funnel, Schlenk tube, gas manifold, glove box);
11.statement of the mass, % purity, and % yield of product collected;
12.if the product is a chiral molecule, then some kind of optical characterization is required such as optical rotation (concentration, solvent specified, temperature), and enantiomeric (diastereomeric) excess or ratio;
13.if the product is a solid, a melting point should be recorded;
14.if the product is a liquid (oil), a distillation boiling point should be recorded;
15.itemization of spectroscopic data: 1H and 13C NMR along with structural assignments; IR peaks along with characteristic functional group absorptions; mass spectrum MW fragments and molecular ion MW;
16.if microwave irradiation is used as a heat source, then the power (Watts), reaction time, reaction temperature, and energy efficiency of the apparatus should be stated; and
17.if continuous flow apparatus is used, then the flow rates, dimensions of tubing and reaction chamber, residence time, and process time should all be stated.
