Entry Substrate Oxidant (equivalent) H2SO4 (%) Time (min) Product Yield 1 1a SbCl5 (2.5) 0.0 30 2a 78 2 1a SbCl5 (2.5) 0.3 30 2a 70 3 1a SbCl5 (2.5) 0.0 180 2a 70 4 1a SbCl5 (3.2) 0.0 30 2a 50 5 1b SbCl5 (2.5) 0.0 30 2b 55 6 1c SbCl5 (2.5) 0.0 30 2c 59 7 3 + 4 SbCl5 (2.5) 0.0 30 5 25 8 1a FeCl3 (2.5) 0.3 30 2a 65 9 1a MoCl5 (2.5) 0.3 30 2a 74 10 1a VOCl3 (2.5) 0.3 30 2a 81

Table 1: Preparation of hexaalkoxy-TPs using SbCl5 in CH2Cl2 solution.