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. 35344-95-7, name is 1H-Pyrazole-4-carbaldehyde, A new synthetic method of this compound is introduced below., Quality Control of 1H-Pyrazole-4-carbaldehyde
To a stirred solution of iFi-pyrazole-4carbaldehyde (1.00 g, 10.41 mmoi) in MeOH (20 mL) was added acetic acid (0.60 mL, 10.41 mrnol), Intermediate 74 (2.59 g, 12.49 mmol) andthe reaction mixture was stirred at ambient temperature for 20 miii. Then NaCNI3H4 (1 .96 g,3 1.2 mmol) was added and stirring was continued at ambient temperature for 14 h. The reaction mixture was distilled under reduced pressure and basified with saturated sodium bicarbonate solution (50 mL). To the resulting aqueous mixture was added BOC2O (2.34 ml, 10.09 mniol) and stirred at ambient temperature for 2. h. The reaction mixture was diluted with water (20 mL) and extracted with 5percent mnethanoi:DCM (3 x 30 mL). The combined organic layers were dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography (Redisep-24 g, 4percent MeOHJCHCI3), to obtainintermediate 721 (095 g, 24.29percent). ?HNMR (300 MHz, DMSO-d6) 8 ppm 1.23 1.46 (in, 9 H)1.57 (s, I H) 2.26 (hr. s., 3 H) 308 – 3.26 (in, I H) 4.21 4.32 (m, 2 H) 5.07 – 5.19 (in, I H) 5.37(s, 2 H) 5.59 -5.71 (m, I H) 7.31 – 7.42 (m, I H) 7.69 (s, 3 H) 12.58- 12.73 (m, I H). LCMS(Method?H;): retention time 1.29 mm. [M-Hj 388.0.
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.