Water → ACRYLAMIDO BUFFER

HRID 462350Notes

Reaction equation

HRID 462350 reaction equation
[C:1](Cl)(=[O:4])[CH:2]=[CH2:3].[CH3:6][N:7]1[CH2:12][CH2:11][NH:10][CH2:9][C:8]1=O.C(=O)([O-])[O-].[Na+].[Na+].O>C(Cl)Cl>[C:1]([N:10]1[CH2:11][CH2:12][N:7]([CH3:6])[CH2:8][CH2:9]1)(=[O:4])[CH:2]=[CH2:3]

Participants

6

Reactant 4

HCID 962WaterHCID 10340Sodium CarbonateHCID 13140Acryloyl chlorideHCID 43990421-Methylpiperazin-2-one

Product 1

HCID 13742939ACRYLAMIDO BUFFER

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent2×

Procedure

Acryloyl chloride (90.5 g) in methylene chloride (100 ml) was added into a methylene chloride (500 ml) solution of N-methyl piperazone (100 g) over a period of one hour. The reaction temperature was kept below 25° C. with cooling. After the addition was completed, the reaction mixture was stirred at ambient temperature for two hours. Then, sodium carbonate (53 g) in 250 ml. of water was added into the reaction mixture with stirring. A crude product (76 g) of 1-acryloyl-4-methyl piperazine was recovered from the methylene chloride solution. The product was distilled and the fraction collected at 65°-69° C./1.5 mm Hg was characterized by I.R. and C13 NMR and was found to be 97% pure by G. C.

Workup

  1. customwas kept below 25° C.
  2. temperaturewith cooling
  3. additionAfter the addition
  4. stirringwith stirring
  5. customA crude product (76 g) of 1-acryloyl-4-methyl piperazine was recovered from the methylene chloride solution
  6. distillationThe product was distilled
  7. customthe fraction collected at 65°-69° C./1.5 mm Hg

Sources & evidence

ORD record
ord-11491c7616d649c0b42bffadbe20ad0b
Source dataset
uspto-grants-1985_05
Patent number
US04515658

Reaction notes

Loading…