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. 444-29-1, name is 1-Iodo-2-(trifluoromethyl)benzene, A new synthetic method of this compound is introduced below., Formula: C7H4F3I
Example 284; (S)-1,4-Dibenzyl-2-[2-(2-trifluoromethyl-phenyl)-ethyl]-piperazine; Combine (S)-1, 4-dibenzyl-2-vinyl-piperazine (6.0 g, 20.52 mmol) and 9- borabicyclo [3.3. 1] nonane (164.1 ml, 82.07 mmol, 0.5 M in THF) and stir at ambient temperature. After 24 hrs, add 1-iodo-2-trifluoromethyl-benzene (8.37 g, 30.78 mmol), triphenylphosphine (861.0 mg, 3.28 mmol), tetrakis (triphenylphosphine) palladium (0) (474.1 mg, 0.41 mmol), and 3N NaOH (16.8 ml) and stir at 60°. After 22 hrs, remove the THF under vacuum and dissolve the residue in ethyl acetate. Wash the organic layer with 1N NaOH then combine, wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Purify the residue using ethyl acetate/hexanes (5: 95) and reduce the appropriate fractions to residue. Stir the residue in 2N NaOH, and extract with diethyl ether. Wash the organic with 1N H2SO4 then adjust the aqueous to pH 14. Extract the aqueous with diethyl ether and combine, wash (brine), dry (sodium sulfate), and reduce the extracts to residue. Recrystallize the residue in warm ethanol to give 2.67 g (30percent) of the title compound: mass spectrum (ion spray): mp 77°-82° ; m/z = 439.2 (M+1) ; Analysis for C27H29F3N2 : calcd: C, 73.95 ; H, 6.67 ; N, 6.39 ; found: C, 74.11 ; H, 6.68 ; N, 6.50.
The synthetic route of 444-29-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ELI LILLY AND COMPANY; WO2003/82877; (2003); A1;,
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