Oxalyl chloride → HCID 22056630, compound

HRID 1923398Notes

Reaction equation

HRID 1923398 reaction equation
Cl.[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([CH2:9][CH2:10][C:11]([OH:13])=O)[CH2:5][CH2:4]1.C(Cl)(=O)C([Cl:17])=O>ClCCl.CN(C)C=O>[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([CH2:9][CH2:10][C:11]([Cl:17])=[O:13])[CH2:5][CH2:4]1

Participants

5

Reactant 2

HCID 65578Oxalyl chlorideHCID 67402292103039-94-7

Product 1

HCID 22056630HCID 22056630, compound

Reagents, catalysts & solvents 2

HCID 6228DimethylformamideCatalystHCID 6344DichloromethaneSolvent

Procedure

A suspension of 3-(1-methylpiperid-4-yl)propionic acid hydrochloride (WO 9620173 A1, Example 1)(0.33 g, 0.00159 mole) in dry dichloromethane (10 ml) was treated with dimethylformamide (1 drop) and oxalyl chloride (0.416 ml, 0.605 g, 0.00477 mole) under an atmosphere of argon. After stirring for 3½ hours the mixture was concentrated in vacuo. The residue was dissolved in dry dichloromethane and concentrated in vacuo to give the title compound as a white solid.

Workup

  1. concentrationwas concentrated in vacuo
  2. dissolutionThe residue was dissolved in dry dichloromethane
  3. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-ccd8cf6f3215490ab2277e3dcf3ced0d
Source dataset
uspto-grants-2012_05
Patent number
USRE043390E1

Reaction notes

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