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. 6940-76-7, name is 1-Chloro-3-iodopropane, A new synthetic method of this compound is introduced below., COA of Formula: C3H6ClI
Example 2; [0060]Synthesis of (4SV3-((2S)-5-chloro-2-r2-(trifluormethv?phenyllpentanovU-4-phenyl-L3- oxazolin-2-one [Formula 36][0061]LHMDS (1 M solution in THF, 94.3 mL, 94.3 mmol) was added dropwise to a solution of the compound of Example 1 (27.5 g, 78.7 mmol) in THF (275 mL) at -15C. 1- Chloro-3-iodopropane (33 mL, 315 mmol) and DMPU (94.8 mL, 787 mmol) were added dropwise thereto at -15C. The mixture was stirred at -150C for 23 hours and at 00C for 15 hours, followed by addition of a 5% sodium chloride solution (275 mL) and MTBE (275 mL). The organic layer was washed with a 5% sodium chloride solution (275 mL) and concentrated under reduced pressure. The residue was extracted with a mixture of MTBE (140 mL) and heptane (140 mL) and with water. The organic layer was concentrated under reduced pressure and then azeotropically distilled with MTBE (55 mL) twice. Ethanol (83 mL) was added to the residue, followed by heating to 500C. After confirming the formation of a homogeneous solution, a small amount of seed crystals were added. After one hour at room temperature, filtration was performed. The crystals were washed with cold ethanol (15 mL) and dried under reduced pressure to obtain 17.5 g of the title compound (content: 92%, 94.6% de) in a yield of 51.3%.Ethanol (48 mL) was added to the resulting title compound (content: 92%, 16 g, 34.6 mmol), and the compound was completely dissolved by heating to 500C. The solution was gradually cooled to room temperature. The generated crystals were washed with cold ethanol (15 mL) and dried under reduced pressure to obtain 14.9 g of the title compound (content: 96.3%, 100% de) in a yield of 97.8%.1H-NMR (400 MHz, CDCl3): delta 1.64-1.72 (m, IH), 1.74-1.84 (m, IH), 1.98-2.09 (m, IH), 2.12- 2.23 (m, IH), 3.44-3.53 (m, 2H), 4.31 (dd, J = 3.2, 8.8 Hz, IH), 4.68 (dd, J = 8.8, 8.8 Hz, IH), 5.36 (dd, J = 3.2, 8.8 Hz, IH), 5.54 (dd, J = 4.8, 9.2 Hz, IH), 7.28-7.34 (m, 2H), 7.35-7.46 (m, 4H), 7.52-7.59 (m, 1 H), 7.60-7.68 (m, 2H).
The synthetic route of 6940-76-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Eisai R&;D Management CO., LTD.; UEMURA, Toshiyuki; SASAKI, Takeo; HOSHINO, Yorihisa; ISOMURA, Minetaka; WO2010/98496; (2010); A1;,
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