Category: 773136-66-6

Adding a certain compound to certain chemical reactions, such as: 773136-66-6, name is Ethyl 2-Fluoro-5-iodobenzoate, belongs to iodides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 773136-66-6, Formula: C9H8FIO2

Under nitrogen atmosphere, starting Ester Intermediate 5e (5.0 g, 15.3 mmol) was dissolved in THF (40 mL), the reaction mixture was cooled to -50C and stirred for 10 minutes. Isopropyl-magnesium-chloride (1 1 mL of a 2M solution in THF) was added dropwise and the reaction mixture was stirred at -50C for 2h. The reaction mixture was cooled to -78C and a solution of cyclobutanone (2.15 g, 30.6 mmol) in THF (10 mL) was added dropwise. The reaction mixture was stirred at -78C for 1 h, then warmed to room temperature and stirred for 18h. The solvent was removed under vacuum, dichloromethane was added and the reaction mixture was washed with a saturated solution of NaHCO3, The organic phase was concentrated under vacuum and the crude product obtained was purified by flash chromatography (eluent from 90:10 to 80:20 Cy/EtOAc) to obtain the desired product (3.0 g). GC-MS (Method 10): Rt = 10.91 min MS : m/z = 210 (M-28)+

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, Ethyl 2-Fluoro-5-iodobenzoate, other downstream synthetic routes, hurry up and to see.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; GIOVANNINI, Riccardo; BERTANI, Barbara; FRATTINI, Sara; DI ANTONIO, Giustino; WO2014/19979; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Application of 773136-66-6, These common heterocyclic compound, 773136-66-6, name is Ethyl 2-Fluoro-5-iodobenzoate, 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.

10586] Under nitrogen atmosphere, starting Ester Intermediate Se (5.0 g, 15.3 mmol) was dissolved inTHF (40 mE), the reaction mixture was cooled to -50 C. and stirred for 10 minutes. Isopropyl-magnesium-chioride (11 mE of a 2M solution in THF) was added dropwise and the reaction mixture was stirred at -50 C. for 2 h. The reaction mixture was cooled to -78 C. and a solution of cyclobutanone (2.15 g, 30.6 mmol) in THF (10 mE) was added dropwise. The reaction mixture was stirred at -78 C. for 1 h, then warmed to room temperature and stirred for 18 h. The solvent was removed under vacuum, dichloromethane was added and the reaction mixture was washed with a saturated solution of NaHCO3, The organic phase was concentrated under vacuum and the crude product obtained was purified by flash chromatography (eluent from 90:10 to 80:20 Cy/EtOAc) to obtainthe desired product (3.0 g).10587] GC-MS (Method 10): R=10.91 mm10588] MS: mlz=210 (M-28)

The synthetic route of 773136-66-6 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; GIOVANNINI, Riccardo; BERTANI, Barbara; FRATTINI, Sara; DI ANTONIO, Giustino; US2014/45856; (2014); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Synthetic Route of 773136-66-6, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 773136-66-6 as follows.

Add NaH (3.71 g, 92.8 mmol, 60.0% purity, 1.3e q) to dry THF (131.0 mL).Compound 2 (21.0 g, 71.4 mmol, 1 eq) and 1-vinylpyrrolidin-2-one (8.49 g, 76.4 mm ol, 8.17 mL, 1.07 eq).The mixture was stirred at 80 C for 3 hours.It was then cooled to room temperature.Then 10% HCl solution (30 mL) was slowly added and stirred at 100 C for 10 hours.The progress of the reaction was detected by TLC (P etroleum ether/Ethyl acetate = 4/1, Rf = 0.68).When the reaction is over,In the condition of an ice bath,Gradually add 1M NaOH solution,The pH of the reaction solution was adjusted to 8.0.Further extraction with DCM (50.0 mL x 2),And by column chromatography (SiO2,Petroleum ether/Ethyl acetate=8/1to 5/1),Obtained white compound 3 (1.60 g, 5.53 mmol,7.75% yield).Figure 4 shows the results of TLC chromatography for this reaction.The NMR data for Compound 3 is:

According to the analysis of related databases, 773136-66-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Shanghai Health Medical School; Tang Dewei; Huang Gang; Huang Chen; Wu Xingyu; Yu Meicen; Li Yanjiao; (18 pag.)CN109942582; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com