Triethylamine → HCID 86734348, compound

HRID 1414158Notes

Reaction equation

HRID 1414158 reaction equation
Cl[CH2:2][CH2:3][C:4]([NH:6][S:7](=[O:15])(=[O:14])[NH:8][C:9](=[O:13])[CH2:10][CH2:11]Cl)=[O:5].C(N(CC)CC)C>CC(C)=O>[C:9]([NH:8][S:7](=[O:14])(=[O:15])[NH:6][C:4](=[O:5])[CH:3]=[CH2:2])(=[O:13])[CH:10]=[CH2:11]

Participants

4

Reactant 2

HCID 8471TriethylamineHCID 86734349HCID 86734349, compound

Product 1

HCID 86734348HCID 86734348, compound

Reagents, catalysts & solvents 1

HCID 180AcetoneSolvent

Procedure

60 g (0.208 mol) of N,N'-bis-(3-chloropropionyl)-sulphuric acid diamide are dissolved in 1 l of absolute acetone. 100 g (0.99 mol) of absolutle triethylamine are added over the course of 15 minutes from a dropping funnel. The mixture is stirred at room temperature until no further precipitate forms and is filtered. The filtrate is concentrated until crystallisation commences. It is then allowed to complete crystallisation at 10°C and after filtration, washing with absolute ether and drying N,N'-bis-acryloyl-(sulphuric acid diamide) mono-triethylamminium salt of melting pont 104°C is obtained. This can be purified further by recrystallisation or can be obtained as free N,N'-bis-acryloyl-sulphuric acid diamide by dissolving in water and acidifying with hydrochloric acid.

Workup

  1. filtrationis filtered
  2. concentrationThe filtrate is concentrated until crystallisation commences
  3. customcrystallisation at 10°C
  4. filtrationafter filtration
  5. washwashing with absolute ether
  6. dry with materialdrying N,N'-bis-acryloyl-(sulphuric acid diamide) mono-triethylamminium salt
  7. customof melting pont 104°C
  8. customis obtained
  9. customThis can be purified further by recrystallisation

Sources & evidence

ORD record
ord-2241f9c35c8944959581306bd509765b
Source dataset
uspto-grants-1977_01
Patent number
US04001201

Reaction notes

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