Continuously updated synthesis method about 4-Chlorobutyl acetate

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.

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. 6962-92-1, name is 4-Chlorobutyl acetate, A new synthetic method of this compound is introduced below., 6962-92-1

To a suspension of sodium ethoxide (4 g, 59.18 mmol) in EtOM (50 mL) was added thiophenol (5 g, 45.45 mrnol) at0C, followed by drop-wise addition of 4-chiorobutyl acetate (7 g, 45.45 minol) over a period of 20 mm. and stirred the same temperature for 10 mm. and heated at reflux for 6 h. The RM was cooled the reaction to RT, added KOH pellets (2.6 g, 45.45 inmol), heated at reflux for4 h. After completion, the RM was poured into ice water, extracted with EtOAc (2 times), EtOAc layer was washed with water, brine, dried over anhydrous Na2SO4, filtered and the solvent was evaporated under reduced pressure to get crude compound. The crude compound was purified by silica gel(60-120 mesh) column chromatography, eluted with 8%EtOAc/pet ether to afford 4-(phenylthio)butan-1-ol as oily mass (6 g, 72%); ?H NMR (400 MHz, cdcl3) 5 7.33 (dd, J = 8.2,1.6 Hz, 2H), 7.30 – 7.23 (m, 2H), 7.20 – 7.14 (m, 1H), 3.65 (td, J = 5.0, 4.1, 3.0 Hz, 2H), 2.96 (t, J = 6.9 Hz, 2H),1.78 – 1.65 (m, 4H); Mass (M+H): 183, LCMS Purity: 99.83%.

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; SUMITOMO CHEMICAL COMPANY, LIMITED; NAKASHIMA, Yosuke; JIN, Yoshinobu; WO2014/84407; (2014); A1;,
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