Reference of 10485-09-3, These common heterocyclic compound, 10485-09-3, name is 2-Bromoindene, its 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.
Tert-butyllithium (48.5 ml, 93.0 mmol, 3 eq.) Was added dropwise to a solution of 2-bromoindene (6.00 g, 31.0 mmol, 1 eq.) In 200 ml of anhydrous ether at -80 C. The resulting mixture was heated to -20 C, and a solution of CuCN (0.27 g, 3.10 mmol, 0.1 equivalent) and LiCl (0.26 g, 6.20 mmol, 0.2 equivalent) in 20 ml of THF was added dropwise. After the solid is completely dissolved, add a portion of chlorodimethyl (2,3,4,5, -tetramethylcyclopenta-2,4-dienyl) silane (6.60 g, 31.0 mmol, 1 equivalent), and The reaction mixture was slowly warmed to a warm temperature and stirred overnight. The resulting mixture was poured into water, the organic layer was separated, and the aqueous layer was extracted with ether. The combined organic phases were dried over anhydrous sodium sulfate and then evaporated to dryness. The residue was purified by preparative HPLC (Waters 2525 pump; Waters 996 PDA detector (UV-Vis); chromatographic column: Phenomenex LinaC18 (2) 50 × 250 mm, 10 um; eluent: MeCN, 100 ml / min). As a yellow oil, 2.30 g (28%) of the title product was obtained.
The synthetic route of 10485-09-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; SABIC Worldwide Technology Co., Ltd.; N ·H·fulaidelichisi; A ·weiduoliya; R ·xipuluo; V ·buxike; I ·bolisuofu; B ·A·gujifu; D ·Y·muladantesaifu; M ·I·xialikefu; D ·wubosiji; A ·wosikebonikefu; H ·keen; (16 pag.)CN110650964; (2020); A;,
Bromide – Wikipedia,
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