2-Chloroethyl methyl ether → HCID 86707687, compound

In an autoclave of 100 mL, N-butyl-N-ethylamine (34.0 g, 390 mmol) was made reacted with chloroethyl methyl ether (18.5 g, 196 mmol) at 130 deg C. for 48 hours. Solid salt that was formed was removed by filtration, and residue (filtrate) was subjected to reduced-pressure distillation by using a Vigreux column of 25 cm. Then 1H-NMR measurement of obtained amine is performed, and it was confirmed that chemical shifts, δ (ppm), are 3.45-3.42 (t, 2H), 3.31(s, 3H), 2.52-2.50(t, 2H), 2.34-2.31(t, 2H), 2.22(s, 3H), 1.45-1.38(m, 2H), 1.31-1.22(m, 2H), and 0.89-0.85(t, 3H), and that N-butyl-N-methyl-N-2-methoxyethylamine was synthesized.

1. customSolid salt that was formed
2. customwas removed by filtration, and residue (filtrate)
3. distillationwas subjected to reduced-pressure distillation

ORD record

ord-1a2f6bbd08044c018e3ac43b0eaff8d1

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09379413B2