Reference of 433-94-3, These common heterocyclic compound, 433-94-3, name is 2-Chloro-6-(trifluoromethyl)aniline, 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.
Preparation 9 2-Chloro-6-trifluoromethyl-phenyl)-hvdrazine hydrochlorideTo a 0 0C solution of 2-chloro-6-trifluoromethyl-phenylamine (35.7 mmol, 7.0 g) in THF (100 mL) is added 48% BF3OEt (143 mmol, 36 mL) followed by addition of isoamyl nitrite (143 mmol, 19 mL). The reaction is stirred for 1 hour and is filtered to collect the tetrafluoroborate diazonium salt (48.7 mmol, 9.0 g). The salt is dissolved in a mixture of cone. HCl (30 mL) and water (10 mL) at 0 0C. To the resulting mixture is added ascorbic acid (48.7 mmol, 8.5 g). The reaction is heated to 50 0C for 3 hours and cooled to room temperature. The solid is filtered and washed with ice water. The wet solid is dissolved in a mixture of cone. HCl (30 mL) and water (20 mL) and heated to 90 0C for 2 hours. The reaction is cooled to 0 0C and filtered to yield the title compound (5.0 g, 60%). LC-ES/MS m/e 157.0 (M+l).
The synthetic route of 433-94-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ELI LILLY AND COMPANY; WO2007/140183; (2007); A1;,
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