반응 #217152

ord-c8dfbb5099684f5fab825c642b5c6da5

반응 방정식

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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The 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
    여과The precipitated product is filtered off with suction
  4. 4
    세척washed repeatedly with isopropanol
  5. 5
    여과The cloudy solution is clarified by filtration with 0.2 g of active charcoal through a pressure
  6. 6
    여과filter

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05470990uspto-grants-1995_11