Electric Literature of 1189352-83-7, A common heterocyclic compound, 1189352-83-7, name is 3-Chloro-5-iodobenzotrifluoride, molecular formula is C7H3ClF3I, 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.
EXAMPLE 6Preparation of 1 -[3-chloro-5-(trifluoromethyl)phenyl]-2,2,2-trifluoroethanone A tetrahydrofuran solution of isopropylmagnesium chloride (2 M, 36.0 mL, 71.8 mmol) was added dropwise to a solution of l-chloro-3-iodo-5-(trifluoromethyl)benzene (i.e. the product of Example 5) (20.0 g, 65.3 mmol) in tetrahydrofuran (30 mL) at -5 0C. The mixture was stirred for 1 h at 0-5 0C. Methyl trifluoroacetate (10.0 g, 78.1 mmol) was added dropwise to the mixture while maintaining the temperature 0-5 0C. When the addition was complete the mixture was stirred for 90 min.Hydrochloric acid (1 N, 100 mL) was added dropwise to the mixture at 0-5 0C. When the addition was complete the mixture was extracted with ether (2 x 100 mL).The combined extracts were dried and evaporated. The oil was dissolved in toluene (55 mL), and /?-toluenesulfonic acid monohydrate (0.100 g, 0.525 mmol) was added to the mixture. The mixture was boiled for 30 min, and the water/toluene methanol/toluene azeotropes were removed by distillation at atmospheric pressure. The distillation was continued at reduced pressure to give the product as an oil (12.4 g, 69% yield), b.p. 93- 103 0C at 6.7 kPa. 1H NMR (CDCl3) 8.21-8.19 (m, 2H), 7.95 (s, IH).
The synthetic route of 1189352-83-7 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; WO2009/126668; (2009); A2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com