Yield:1178819-40-3 87.4%

Reaction Conditions:

at 120; for 16 h;Product distribution / selectivity;autoclave;

Steps:

1.1

Preparation Examples1. Preparation of N-(2,2-difluoroethyl)prop-2-en-1-amine (step (i)) Example 1.1An amount of 382 g (3.67 mol) of 2,2-difluoro-1-chloroethane and 70 g (1.2 mol) of prop-2-en-1-amine are heated in an autoclave at 120° C. for 16 hours. The reaction mixture is treated with 200 g of water and the phases are subsequently separated. The organic phase is distilled at 55° C. An amount of 65 g of N-(2,2-difluoroethyl)prop-2-en-1-amine is obtained (corresponds to 87.4% yield, based on reacted prop-2-en-1-amine). Unreacted prop-2-en-1-amine, which precipitates as hydrochloride, can be rereleased by addition of sodium hydroxide solution.¹H NMR (CDCl₃): 5.76-6.0 (m, 2H), 5.22 (m, 1H), 3.31 (m, 2H), 2.96 (dt, 2H)

References:

US2012/142971,2012,A1 Location in patent:Page/Page column 5