The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings.
Related Products of 52548-14-8,Some common heterocyclic compound, 52548-14-8, name is 2-Iodo-5-methylbenzoic acid, molecular formula is C8H7IO2, 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.
EXAMPLE EMethyl 2-iodo-5-methylbenzoate (E-I) A visually clean 100 L flask equipped with a mechanical stirrer thermocouple and water chilled condenser was charged with MeOH (50 L). 2-iodo-5-methylbenzoic acid (5.85 kg, 22.32 mol) was then added while stirring. Concentrated sulfuric acid (0.595 L, 11.16 mol) was then added portion- wise which caused an increase in temperature from 17 0C to 22 0C. This mixture was gradually brought to an internal temperature of 64.6 0C an aged overnight (~18h). The next morning the reaction had reached >98% conversion by HPLC. The flask was cooled to 160C by placing in an ice bath and 850ml of ION NaOH (0.98 equiv.) was added slowly (over 10 minutes) while monitoring the pH. After the addition the pH was 5-6 (Caution: bringing pH over 9 can result in saponification during the work-up). The solution was then concentrated to about 16L and this suspension was transferred to a 100 L extractor. The flask was rinsed with 8L of IPAc and 4L of water which were also transferred to the extractor. 32L IPAc along with 1OL of 5w% NaHCO3 and ~10L of 15w% Brine. The layers were cut and the aqueous layers were back- extracted with 2OL of IPAc. The organic layers were then combined and washed with 1OL of 15w% Brine. The organic layers were collected to provide E-I (6.055 kg, 21.93 mol, 98 % yield) in 98.3% purity.
The synthetic route of 52548-14-8 has been constantly updated, and we look forward to future research findings.