Synthesis
The general procedure for the synthesis of ethyl 4-methyl-1hydro-indole-2-carboxylate from the compound (CAS: 24512-97-8) was as follows: 19.5 g (0.0844 mol) of the azide prepared in step 1 was added in batches to 100 mL of xylene preheated to 140 °C. After the addition was completed, the reaction mixture was kept at 140 °C for 1 hour. At the end of the reaction, the xylene was removed by concentration via reduced pressure distillation, and the residue was dissolved in isopropyl ether, filtered, and dried under vacuum at 40 °C for 18 h to give a white crystalline product. The melting point of the product was 141 °C and the yield was 62%.
References
[1] Journal of the Chemical Society, Chemical Communications, 1982, # 1, p. 3 - 4
[2] Patent: US2004/43995, 2004, A1. Location in patent: Page 13
