Category: chlorides-buliding-blocks

14752-66-0, A common heterocyclic compound, 14752-66-0, name is Sodium 4-chlorobenzenesulfinate, molecular formula is C6H4ClNaO2S, 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.

General procedure: A mixture of alkyne 1 (0.25 mmol), sodium sulfinate 2 (0.375 mmol), FeCl3 (20 mol %),K2S2O8 (20 mol %), and water (3 mL) was stirred at rt in an open flask for 6-9 h(Table 2). After completion of the reaction (monitored by TLC), the mixture was extracted with EtOAc (3 5 mL). The combined organic phases were dried over anhyd. Na2SO4, filtered, and concentrated under reduced pressure. The resulting crude product was purified by silica gel column chromatography using a mixture of EtOAc-n-hexane (1:4) as eluent to afford an analytically pure sample of beta-keto sulfones 3 (Table 2).

The synthetic route of 14752-66-0 has been constantly updated, and we look forward to future research findings.

Reference:
Article; Singh, Atul K.; Chawla, Ruchi; Yadav, Lal Dhar S.; Tetrahedron Letters; vol. 55; 17; (2014); p. 2845 – 2848;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics

As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 6940-78-9 name is 1-Bromo-4-chlorobutane, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below. 6940-78-9

(1) 3.53 g (20.6 mmol) of 1-bromo-4-chlorobutane was dissolved in 50 ml of absolute ethanol, added to a 250 ml round bottom flask, stirred in an ice bath at 0 C. A constant pressure dropping funnel was slowly added dropwise to a solution containing 3.11 g (22.2 mmol, 1.08 times) of 50% sodium thiomethoxide in anhydrous ethanol, and the temperature was gradually raised to room temperature overnight. The total reaction time was 26 hours. Stirring was carried out, and the ethanol was removed by vacuum at low temperature and extracted three times with n-hexane. The mixture was washed with saturated sodium chloride and dried over anhydrous sodium sulfate. The insoluble material was filtered off. Vacuum at low temperature steaming to remove n-hexane, with a strong mustard odor of 2.69g of colorless oil. The intermediate content of GC-MS was about 81%, and the yield of intermediate was about 76.3%.

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-4-chlorobutane, and friends who are interested can also refer to it.

Reference:
Patent; Shenyang Pharmaceutical University; Sun, Lixin; Li, Binglong; Zhou, Hui; (10 pag.)CN106496086; (2017); A;,
Chloride – Wikipedia,
Chlorides – an overview | ScienceDirect Topics