These common heterocyclic compound, 29027-20-1, name is 3-Chloro-5-methylaniline, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Quality Control of 3-Chloro-5-methylaniline
Triphosgene (17.01 g, 0.0573 mol) was dissolved in 200 ml of tolunen in a 1 liter flask. 150 ml of a toluene solution of 3-chloro-5-methylaniline (21.9 g, 0.155 mol) and triethylamine (36.0 ml) was added dropwise thereto over 30 minutes at room temperature. The reaction mixture was then stirred at 70° C. for 2 hours and cooled to room temperature. The obtained precipitates of hydrochloric acid salt of triethylamine were filtered out and the filtrate liquid was concentrated and treated with distillation at a reduced pressure to obtain 16.87 g of a colorless liquid (production yield 65%). B.p.: 72-74° C./0.53-0.66 kPa (4-5 torr) 1H-NMR, 500 MHz, in CDCl3 (delta) 7.00 (bs, 1H), 6.90 (bs, 1H), 6.80 (bs, 1H), 2.31 (s, 3H)
The synthetic route of 3-Chloro-5-methylaniline has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Ichida, Akito; US2004/147776; (2004); A1;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics