ChemicalBook CAS DataBase List Fenfluramine hydrochloride

Fenfluramine hydrochloride synthesis

6synthesis methods

Product Name:Fenfluramine hydrochloride
CAS Number:404-82-0
Molecular formula:C12H17ClF3N
Molecular Weight:267.72

21906-39-8 Synthesis

21906-39-8
190 suppliers
$8.00/1g

557-66-4 Synthesis

557-66-4
267 suppliers
$28.00/25g

404-82-0
4 suppliers
$24.00/1mg

Yield:404-82-0 148 g

Reaction Conditions:

Stage #1: ethanamine hydrochloridewith sodium hydroxide in methanol at 0 - 15; for 0.5 h;
Stage #2: 3-(trifluoromethyl)phenylacetone in methanol at 0 - 5; for 0.5 h;Further stages;Reagent/catalyst;Temperature;

Steps:

4 Example-4: Preparation of compound of formula-la.

Around bottom flask was charged with sodium hydroxide (112 g ), methanol (528 mL) stirred at 0-5 °C for 15 min. Ethylamine hydrochloride (225 g) was added to the above reaction mixture at same temperature and stirred for 30 min. A compound of formula-4 (160 g ) was added to the reaction mass at 0-5 °C and stirred for 30 min. Sodium borohydride (28.8 g) was added portion wise to the above reaction mixture keeping the temperature below 10 °C and stirred for 30 min. The reaction mixture was warmed to 20-25°C, stirred for 5 hours. Methanol was distilled off under reduced pressure below 40°C, added water (650 mL), dichloromethane (350 mL) stirred for 15 min. The organic layer was separated, washed with water (200 mL x 3) and the organic layer was evaporated to get Fenfluramine free base as colorless oil (160 g). The obtained Fenfluramine crude compound (160 g) was diluted with ethyl acetate (1200 mL), adjusted the p^H upto 1.0 by using isopropyl alcohol hydrochloride (245 mL) at 0-5 °C and stirred for 30 min. The reaction mixture was warmed to 25-30 °C and stirred for 1 hr, the obtained solid was filtered and dried to obtain the title compound. (0058) Yield : 148 g . (0059) Purity by HPLC: >99.9 %

References:

WO2021/117057,2021,A1 Location in patent:Page/Page column 10-12

713-45-1 Synthesis