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. Author manuscript; available in PMC: 2014 Jul 29.
Published in final edited form as: Nat Protoc. 2013 May 2;8(6):1042–1047. doi: 10.1038/nprot.2013.059

Table 1.

Troubleshooting table.

Step Problem Possible reason Solution
8 The obtained solution is cloudy. Inorganic salts (including Zn) may be present. Repeat Steps 7 and 8 using more sand; alternatively, use Celite® instead of sand.
12 Water droplets are visible in the flask. Too much water is left in the product. Fix/obtain new vacuum pump; add toluene and repeat evaporation in vacuo.
13/20 Excessively high yields of the desired crude salt. Too much water is left in the product. Fix/obtain new vacuum pump; add toluene and repeat evaporation in vacuo.
13/20 /26 Low yields of the desired crude salt. Starting materials are not pure. Check the purity of the starting materials, repurify them if necessary.
26 Elemental analysis shows %Cl of more than a few % for TFMS (1), DFMS (2) and TFES (3). ZnCl2 was not fully removed from the product. Repeat wash with 1:1 EtOAc:CH2Cl2. For TFES (3), the impure product can be sonicated in the presence of 1:1 EtOAc:CH2Cl2 to help remove more chloride.