Reaktion #217152

ord-c8dfbb5099684f5fab825c642b5c6da5

Reaktionsgleichung

O=S(=O)(O)Cl
sulfochloride
O
water
OCCN(CCO)CCO
triethanolamine
Cl.OCCN(CCO)CCO
triethanolamine hydrochloride

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe excess solvent is substantially removed in vacuo at 120°-150° C.
  2. 2
    workup.ADDITION50 ml of isopropanol are added to the viscous residue
  3. 3
    FiltrationThe precipitated product is filtered off with suction
  4. 4
    Waschenwashed repeatedly with isopropanol
  5. 5
    FiltrationThe cloudy solution is clarified by filtration with 0.2 g of active charcoal through a pressure
  6. 6
    Filtrationfilter

Vorschrift

A suspension of 3.7 g of the sulfochloride of the formula (7) in 15 g of triethanolamine and 3 g of water is stirred at 150° for one hour. The excess solvent is substantially removed in vacuo at 120°-150° C., and 50 ml of isopropanol are added to the viscous residue. The precipitated product is filtered off with suction, washed repeatedly with isopropanol and taken up in approx. 40 ml of water. The cloudy solution is clarified by filtration with 0.2 g of active charcoal through a pressure filter. This gives an aqueous solution of the bistriethanolamine salt of the formula ##STR16## which still contains triethanolamine hydrochloride.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05470990uspto-grants-1995_11