Reference of 137049-00-4, The chemical industry reduces the impact on the environment during synthesis 137049-00-4, name is 1-Methyl-1H-imidazole-4-sulfonyl chloride, I believe this compound will play a more active role in future production and life.
Intermediate 27 (40 mg, 79 mumol) was dissolved in 1 mL of pyridine and flushed with nitrogen, It was cold to 0 C. and added 1-methyl-1 H-imidazole-4-sulfonyl chloride (43,mg, 240 mumol). The mixture was allowed to warm to room temperature and stirred for 20 h under nitrogen. The reaction was diluted with 10 mL of EtOAc, washed with brine, dried over Na2SO4 and concentrated in vacuum to give crude product which was then purified by flash chromatography on silica gel (20% to 50% ethyl acetate in hexane, then 5/5/1 of EtOAc/hexane/MeOH) to provide 55 (24 mg, 47%). m/z=648 (M+1). The deprotection of the DPM group at C8-OH was carried out as in the conversion of 28 to 29. The resulting residue was then purified by reverse-phase prep HPLC to provide 13 mg (59% in yield) of 56 as a TFA salt. 300 MHz 1H NMR (CDCl3) delta (ppm): 9.0 (d, 1H); 8.4 (d, 1H); 7.5 (m, 1H); 7.4 (s, 1H); 7.3 (m, 2H); 7.2 (s, 1H); 7.0 (t, 2H); 4.8 (s, 2H); 4.3-4.5 (m, 2H); 3.6 (s, 3H); 3.4 (s, 3H). m/z=482 (M +1).
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 1-Methyl-1H-imidazole-4-sulfonyl chloride, other downstream synthetic routes, hurry up and to see.