无水无氧基本实验架设-(Schlenk Lines真空线).pdfVIP

Basic Reaction Setup Equipment Reaction flask Stir bar or mechanical stirrer (paddle) Magnetic stir motor or mechanical stir motor Glass gas inlet Addition funnel Rubber septum N inlet/mercury bubbler 2 Procedure: Set up as shown in the figure below. (Variations include using a magnetic stirrer, two-necked flasks, etc.) Flush reaction flask and addition funnel with N2. Add reagent and solvent to reaction flask. Chill or warm as appropriate. Syringe, pour, or cannulate reagent into the addition funnel. If more than one reagent is to be added to the reaction mixture, wash the funnel with solvent between additions. When the last reagent has been added, replace the addition funnel with a glass stopper. rubber septum mechanical stirrer addition funnel to N line 2 Bowl for ice or dry ice bath 16 Filtering in an Airless System Purpose: To remove unwanted solids from a reaction mixture. Equipment: Flask containing reaction mixture with solids Fritted filter with ground glass joints Adapter with hose adapter to connect to N /vacuum line 2 Receiving flask with stir bar Dry ice/acetone bath (-78 °C) Rubber septum Procedure: Set up system as shown in figure. Connect to the vacuum system and evacuate for ca. 5 min. Then fill with N2. Co