反应 #217152

ord-c8dfbb5099684f5fab825c642b5c6da5

反应方程式

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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The 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
    过滤The precipitated product is filtered off with suction
  4. 4
    洗涤washed repeatedly with isopropanol
  5. 5
    过滤The cloudy solution is clarified by filtration with 0.2 g of active charcoal through a pressure
  6. 6
    过滤filter

实验过程

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05470990uspto-grants-1995_11