反応 #441776

反応方程式

potassium carbonate

2,3,5,6-tetrachloro-4-pyridinol

isocyanatoethyl propionate

acetone

→

(2-(1-oxopropoxy)ethyl)carbamic acid

溶媒

n-hexane

反応条件

後処理

1. 1
   温度at reflux temperature for eight hours
2. 2
   workup.STIRRINGThe mixture was again stirred
3. 3
   温度at reflux temperature for an additional seven hours
4. 4
   workup.STIRRINGThe reactants were then stirred for another hour after which the insoluble components
5. 5
   ろ過were filtered off
6. 6
   その他the solvent removed under reduced pressure
7. 7
   その他leaving a residue
8. 8
   温度cooled
9. 9
   ろ過filtered

実験手順

11.7 Grams of 2,3,5,6-tetrachloro-4-pyridinol, 7.2 grams of isocyanatoethyl propionate, and a few drops of dibutyltin dilaurate (as activating agent) were added to 200 ml of acetone and stirred at reflux temperature for eight hours and then allowed to stand. The mixture was again stirred at reflux temperature for an additional seven hours before the addition of 6.0 grams of potassium carbonate. The reactants were then stirred for another hour after which the insoluble components were filtered off and the solvent removed under reduced pressure, leaving a residue. The resulting residue was slurried in n-hexane, cooled, and filtered to yield about 15 grams of soft, white solid as the desired 2,3,5,6-tetrachloro-4-pyridinyl ester of (2-(1-oxopropoxy)ethyl)carbamic acid.

出典