Sodium Iodide → Methyl(2-(piperidin-1-yl)ethyl)amine

A solution of 8.0 g of N-(2-chloroethyl)piperidine hydrochloride and 0.5 g of sodium iodide in 60 ml of methanol which contained 40% of methylamine was reacted at 70° C. in a sealed tube for 20 hours. After allowing the reaction mixture to cool down, the reaction mixture was concentrated under reduced pressure. The residue was added with ether, followed by a further addition of 10 g of ground sodium hydroxide. The resulting mixture was stirred for 2 hours. The insoluble material was filtered off and the filtrate was concentrated under the atmospheric pressure. The residue was distilled under reduced pressure to give 4.5 g of a fraction at 80° C./18 Torr (yield: 73%).

1. customwas reacted at 70° C. in a sealed tube for 20 hours
2. temperatureto cool down
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. additionThe residue was added with ether
5. additionfollowed by a further addition of 10 g of ground sodium hydroxide
6. filtrationThe insoluble material was filtered off
7. concentrationthe filtrate was concentrated under the atmospheric pressure
8. distillationThe residue was distilled under reduced pressure
9. customto give 4.5 g of a fraction at 80° C./18 Torr (yield: 73%)

ORDレコード

ord-50a24f73a84448bdaee945495527e333

出典データセット

uspto-grants-1988_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04762927