Category: 17715-70-7

Adding a certain compound to certain chemical reactions, such as: 17715-70-7, name is 2,4-Dimethoxy-1-fluorobenzene, belongs to ethers-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 17715-70-7, HPLC of Formula: C8H9FO2

A solution of 1-fluoro-2,4-dimethoxybenzene (0.25 g, 1.60 mmol) in 5 mL of CH2Cl2 under Ar atmosphere was cooled to 0 C, then TiCl4 (neat, 0.38 mL, 3.52 mmol) was slowly added. The reaction mixture was left to react for 30 min. Dichloromethyl methyl ether (0.21 mL, 2.40 mmol) was added and the mixture left to react for a further 30 min. The reaction was quenched by the addition of saturated aq. NH4Cl (10 mL) and diluted with CH2Cl2 (10 mL). The mixture was left to stand for 30 min and the organic phase was separated and washed with 0.1 M HCl, saturated aq. NaHCO3 and brine. The organic layer was dried with Na2SO4, filtered and concentrated in vacuo to give crude product which was purified by PTLC with 30% EtOAc/hexanes as eluent to give 5-fluoro-2,4-dimethoxybenzaldehyde as a white solid (0.24 g, 1.30 mmol, 88 %).

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Reference:
Article; Radomkit, Suttipol; Sarnpitak, Pakornwit; Tummatorn, Jumreang; Batsomboon, Paratchata; Ruchirawat, Somsak; Ploypradith, Poonsakdi; Tetrahedron; vol. 67; 21; (2011); p. 3904 – 3914;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 17715-70-7, name is 2,4-Dimethoxy-1-fluorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 2,4-Dimethoxy-1-fluorobenzene

Preparation 29 6-Fluoro-7-hydroxychroman-4-one A mixture of 1,3-dimethoxybenzene (3.80 mL, 29.0 mmol) and N-fluorodibenzenesulfonamide (4.21 g, 29.21 mmol) was heated at 60 C. overnight. The mixture was cooled and flash chromatographed on silica gel (2*5 inches packed in hexane) with elution proceeding as follows: 3% ethyl acetate/hexane (1000 mL), discarded forerun; 3% ethyl acetate/hexane (1000 mL), 2.69 g of a 2:1 mixture of 2,4-dimethoxyfluorobenzene and starting material which was carried directly into the next step. The product of the above reaction was combined with acetic acid (11 mL) and 48% HBr (11 mL) and refluxed 3 h. The reaction was concentrated and flash chromatographed on silica gel (2*5 inches packed in hexane) with elution proceeding as follows: 10% ethyl acetate/hexane (2000 mL), 0.95 g (43%) of 2,4-dihydroxyfluorobenzene as a waxy white solid which was used without purification. A mixture of 2,4-dihydroxyfluorobenzene (0.15 g, 1.17 mmol), 3-chloropropionic acid (0.13 g, 1.20 mmol) and trifluoromethanesulfonic acid (1 mL) were heated to 80 C. for 3 h. The reaction was poured into water and extracted with ether (3x). The combined organic phase was washed with water and brine, dried over magnesium sulfate, and concentrated to give 2,4-dihydroxy-5-fluoro-beta-chloropropiophenone as a red solid which had: NMR delta7.37 (d, J=10.8 Hz, 1 H), 6.54 (d, J=7.7 Hz, 1 H), 3.87 (t, J=6.8 Hz, 2 H), 3.33 (t, J=6.8 Hz, 2 H). This product still contained some residual 3-chloropropionic acid but was suitable for use in the next reaction.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Pfizer Inc.; US6258827; (2001); B1;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

Electric Literature of 17715-70-7,Some common heterocyclic compound, 17715-70-7, name is 2,4-Dimethoxy-1-fluorobenzene, molecular formula is C8H9FO2, 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.

Preparation 29 6-Fluoro-7-hydroxychroman-4-one A mixture of 1,3-dimethoxybenzene (3.80 mL, 29.0 mmol) and N-fluorodibenzenesulfonamide (4.21 g, 29.21 mmol) was heated at 60 C. overnight. The mixture was cooled and flash chromatographed on silica gel (2*5 inches packed in hexane) with elution proceeding as follows: 3% ethyl acetate/hexane (1000 mL), discarded forerun; 3% ethyl acetate/hexane (1000 mL), 2.69 g of a 2:1 mixture of 2,4-dimethoxyfluorobenzene and starting material which was carried directly into the next step. The product of the above reaction was combined with acetic acid (11 mL) and 48% HBr (11 mL) and refluxed 3 h. The reaction was concentrated and flash chromatographed on silica gel (2*5 inches packed in hexane) with elution proceeding as follows: 10% ethyl acetate/hexane (2000 mL), 0.95 g (43%) of 2,4-dihydroxyfluorobenzene as a waxy white solid which was used without purification. A mixture of 2,4-dihydroxyfluorobenzene (0.15 g, 1.17 mmol), 3-chloropropionic acid (0.13 g, 1.20 mmol) and trifluoromethanesulfonic acid (1 mL) were heated to 80 C. for 3 h. The reaction was poured into water and extracted with ether (3*). The combined organic phase was washed with water and brine, dried over magnesium sulfate, and concentrated to give 2,4-dihydroxy-5-fluoro-beta-chloropropiophenone as a red solid which had: NMR delta 7.37 (d, J=10.8 Hz, 1 H), 6.54 (d, J=7.7 Hz, 1 H), 3.87 (t, J=6.8 Hz, 2 H) 3.33 (t, J=6.8 Hz, 2 H). This product still contained some residual 3-chloropropionic acid but was suitable for use in the next reaction.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2,4-Dimethoxy-1-fluorobenzene, its application will become more common.

Reference:
Patent; Pfizer Inc.; US6046213; (2000); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem

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 17715-70-7 as follows. category: ethers-buliding-blocks

Example 15 Preparation of 4-fluororesorcinol (15) Using general method E, Compound 11 (27.4 g, 157.9 mmol) gives Compound 15 as 20.7 g (100%) of a colorless crystalline solid: m.p. 94-96 C.; 1 H-NMR (d6 -DMSO) 8.39 (br, 1H), 8.00 (br, 1H), 6.89 (dd, 1H), 6.48 (dd, 1H), 6.27 (ddd, 1H). 19 F-NMR (d6 -DMSO) 145.82 (m). Anal calc. for C6 H5 FO2: C, 56.26; H, 3.93. Found: C, 56.23; H, 3.93.

According to the analysis of related databases, 17715-70-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Molecular Probes, Inc.; US6162931; (2000); A;,
Ether – Wikipedia,
Ether | (C2H5)2O – PubChem