Sodium Carbonate → HCID 43422974, compound

HRID 494012Notes

Reaction equation

HRID 494012 reaction equation
[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[C:9](Cl)(=[O:12])[CH:10]=[CH2:11].C(=O)([O-])[O-].[Na+].[Na+]>ClCCl.O>[CH3:1][N:2]1[CH2:8][CH2:7][CH2:6][N:5]([C:9](=[O:12])[CH:10]=[CH2:11])[CH2:4][CH2:3]1

Participants

6

Reactant 3

HCID 10340Sodium CarbonateHCID 13140Acryloyl chlorideHCID 2283491-Methylhomopiperazine

Product 1

HCID 43422974HCID 43422974, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent2×

Conditions

Temperature
0 °C

Procedure

A solution is prepared of 20 g (175 mM) of N-methylhomopiperazine in 100 ml of dichloromethane, to which is added, dropwise, at 0° C., a solution of 15.85 g (175 mM) of acryloyl chloride in 20 ml of dichloromethane. The reaction mixture is agitated for 1 hour at 0° C., and then for 2 hours at ambient temperature, and then hydrolysed with a solution of 12 g of sodium carbonate in 20 ml of water. The mixture is decanted, the organic phase is washed once with water and then dried over magnesium sulphate and concentrated under reduced pressure. 23 g of the compound sought after are thus obtained, as an orangy oil, which is used, without other purification, in the next step.

Workup

  1. additionis added
  2. customat 0° C.
  3. waitfor 2 hours at ambient temperature
  4. customThe mixture is decanted
  5. washthe organic phase is washed once with water
  6. dry with materialdried over magnesium sulphate
  7. concentrationconcentrated under reduced pressure
  8. customafter are thus obtained, as an orangy oil, which
  9. customis used, without other purification, in the next step

Sources & evidence

ORD record
ord-cd31acafec7546caa8ff9ca073122838
Source dataset
uspto-grants-2009_05
Patent number
US07538111B2

Reaction notes

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