65412-03-5,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.65412-03-5,4-(2-Aminoethyl)tetrahydro-2H-pyran,as a common compound, the synthetic route is as follows.
Place 2- (4-FORMYLPHENOXY) thiazole-5-carboxamide (Example 12, Part D) (0.187 g, 0.755 MMOL), 2-(tetrahydropyran-4-yl)ethylamine (0.101 g, 0.831 mmol) and 3A molecular sieves in a vial. Add methanol (3.8 mL), cap and stir overnight. Add NaBH4 (0.029 g, 0.755 mmol) and stir until the gasses stop evolving. Load the reaction mixture directly onto a 25 g ISCOO pre-load column. Dry the column in a vacuum oven at room temperature. Purify by eluting through a 40 g LSCO) column with 10% (2. 0 M NH3 in methanol) in ethyl acetate over 45 minutes to give the title compound as a free base. Dissolve the compound in dichloromethane: methanol (2 : 1) (3 mL) and add 1 equivalent of 0.50 M methanesulfonic acid in dichloromethane. Stir the solution for a short time before concentrating to give the title compound: TOF MS ES+ 362.1 (M+H) +, HRMS calcd for CL8H24N303S 362. 1538 (M+H) +, found 362.1536, time 0.32 min ; HPLC [YMC- Pro pack C-18 (150 x 4.6 mm, S-5 MICRON1), 0.05% TFA/acetonitrile in 0.05% TFA/water at 1. 0 ML/MIN, 10-20% OVER 5 min, 20-95% over 18], tR = 8. 0 min, 95. 0% purity.
65412-03-5 4-(2-Aminoethyl)tetrahydro-2H-pyran 2773198, aTetrahydropyrans compound, is more and more widely used in various fields.
Reference£º
Patent; ELI LILLY AND COMPANY; WO2004/80996; (2004); A1;,
Tetrahydropyran – Wikipedia
Tetrahydropyran – an overview | ScienceDirect Topics