Sodium Hydroxide → N,N,N-Trimethyl-3-(methylamino)propan-1-aminium bromide

To a stirred suspension of 876.0 g. (3.0 moles) of N,N,N-trimethyl-[3-(methylamino)]-1-propanaminium bromide hydrobromide in 2.75 liters of absolute methanol at room temperature is added a freshly prepared solution of sodium hydroxide (120.0 g., 3.0 moles) in 1.0 liter of absolute methanol over a period of 1.0 hour. The reaction mixture is evaporated under reduced pressure and the solid residue is shaken with 750 ml. of acetonitrile. The insoluble sodium bromide is removed by filtration and the filtrate is evaporated. The solid residue is dried in vacuo to give a quantitative yield of white, crystalline hygroscopic product which may be used without further purification or can be recrystallized from isopropanol-ether. NMR (D2 0)γ: 2.28 (3H, S, --NHCH3); 3.11 (9H, S, --N+(CH3)3).

1. additionTo a stirred suspension of 876.0 g
2. customThe reaction mixture is evaporated under reduced pressure
3. customThe insoluble sodium bromide is removed by filtration
4. customthe filtrate is evaporated
5. customThe solid residue is dried in vacuo
6. customto give a quantitative yield of white, crystalline hygroscopic product which
7. custommay be used without further purification
8. customcan be recrystallized from isopropanol-ether

ORDレコード

ord-baa1cda78dfe4aa8a582c76a68a40a78

出典データセット

uspto-grants-1980_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04205064