Piperidine → HCID 22048494, compound

HRID 2209328Notes

Reaction equation

HRID 2209328 reaction equation
[NH:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH3:7][O:8][CH2:9][CH2:10]Cl>>[CH3:7][O:8][CH2:9][CH2:10][N:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

3

Reactant 2

HCID 8082PiperidineHCID 123162-Chloroethyl methyl ether

Product 1

HCID 22048494HCID 22048494, compound

Procedure

In an autoclave of 100 mL, piperidine (40.0 g, 470 mmol) was made reacted with chloroethyl methyl ether (22.0 g, 232 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 3.49-3.46 (t, 2H), 3.31(s, 3H), 2.51-2.48(t, 2H), 2.40-2.36(m, 4H), 1.59-1.53(m, 4H), and 1.42-1.36(m, 2H), and that N-2-methoxyethylpiperidine was synthesized.

Workup

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

Sources & evidence

ORD record
ord-bd3d2cb5677040948704c8e505d2736d
Source dataset
uspto-grants-2016_06
Patent number
US09379413B2

Reaction notes

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