Guidelines for Writing Experimental Procedures

Contributed by Dominic McGrath
University of Arizona

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Experimentals

A: Write a fully detailed procedure.

B: Write a fully detailed procedure. Preface with "Compound 36 was prepared as follows:" The reference is to the previous literature report of the compound.

C: Write an abbreviated procedure as follows with only stoichiometry and purification details.

Example: "(R,R)-1-(3',4'-Dibenzyloxyphenyl)-2-(carboethoxy)-1,2-ethanediol (24). Following the procedure for 23, K3Fe(CN)6 (43.0 g, 0.13 mol), K2CO3 (18.1 g, 0.13 mol), K2[OsO2(OH)4] (0.16 g, 0.44 mmol, 1 mol%), (DHQD)2PHAL (343 mg, 0.44 mmol, 1 mol%), methanesulfonamide (4.1 g, 43 mmol), and tert-butyl alcohol (130 mL), water (220 mL), toluene (130 mL), and 22 (16.9 g, 43.4 mmol) yielded 24 (16.7 g, 91%, >99% ee) as a colorless solid after flash chromatography (SiO2, 3:2 petroleum ether-ethyl acetate):"

D: Write a fully detailed procedure. Preface with "A procedure from the literature9 was modified as follows: "

E: Write an abbreviated procedure as shown in C, although the preface is now: "Following a procedure reported in the literature,5 "

F: Write a fully detailed procedure. Preface with "A procedure was adapted from the literature8 as follows:"

G: Do not write an experimental. List the compound in the General Experimental section thusly: "Compound 89 was prepared according to the literature."

 

Characterization Data

X: Provide full characterization data including (at a minimum!) 1H and 13C NMR, combustion analysis, mass spec (EI for small molecules, FAB, electrospray, or MALDI for dendrimers), and, for optically enriched compounds, optical rotation. Note that characterization data follows the experimental isolation and purification of the compound with a colon!..Follow other punctuation in the following example exactly!!!

Example: "1H NMR: d 8.82 (s, 3H), 7.39-7.26 (m, 30H), 6.61 (d, J = 2.2 Hz, 6H), 6.53 (t, J = 2.2 Hz, 3H), 5.02 (s, 12H), 4.74 (d, J = 8.6 Hz, 3H), 4.54 (dd, J = 12.1, 2.9 Hz, 3H), 4.41 (dd, J = 12.1, 5.4 Hz, 3H), 4.09 (ddd, J = 8.6, 5.4, 2.9 Hz, 3H), 1.53 (s, 9H), 1.49 (s, 9H); 13C NMR: d 164.5, 160.2, 139.7, 136.6, 134.9, 131.0, 128.5, 128.0. 127.5, 110.1, 105.6, 101.9, 80.8, 79.5, 70.1, 64.0, 27.0; MS (MALDI) m/z 1439.3 (M+Na), 1456.3 (M+K); [a]= +25.1 (c = 0.62, CH2Cl2). Anal. Calcd for C87H84O18: C, 73.71; H, 5.97. Found: C, 73.81; H, 6.26."

Y: Limited characterization data is necessary. At the minimum you should have a 1H NMR and, in the case of a solid, a melting point. Give the literature value for the melting point after your reported value: "mp 90-91 °C (lit60 90-92 °C)"