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E2: Recrystallization and MPD of CBA

Hot filtration Melting point determination

-fluted filter paper must NOT exceed funnel -capillary tube
-heated receiving E. flask (hot plate on) a. CLOSED in oil bath
-wide bore, short stemmed funnel b. 2-4 mm height sample
-little amount of solvent on E. flask c. attached via rubber tubing
-compound must only be partially submerged
Filter paper -thermometer thru a cork
-Fluted: recrystallization,filtering solvent w/ CBA a. graduation must be seen
-3:1 : cold filtration, washing w/ cold H2O -oil bath
-hot plate turned ON
E3: Purification and Extraction of Caffeine

Solvent extraction (sep. funnel)

-support ring + stand Sublimation set-up
-cap slightly open to allow separation -beaker COVERED with pre-weighed filter
-stopcock: paper, SEALED with rubber band
a. open: parallel to funnel -only 1/3 of beaker immersed in bath
b. closed : perpendicular to funnel -thermometer
c. organic (top); aqueous (bottom) -hot plate turned ON
E4: Paper Chromatography
Paper chromatography
-whatman filter paper #1
- -spot CONCENTRATED, not exceeding 2 mm
- -cork stopper must be covered
a. paperclip, filter paper hanging
- -lines drawn in PENCIL
- -solvent below starting line (0.5-1mm)
- -solvent must not pass thru finish line
-Rf = distance solute/distance solvent
-closed system
-sacrificial paper (ideally)

E6: Synthesis of Tert-butyl Chloride

Separatory funnel – mixing

-perpendicular stopcock
-invert, swirl
-open stopcock to release pressure (3x)

Simple distillation
-receiving flask in ICE bath
-water in NEAR receiving flask
-thermometer just below the side-arm of the
distillation head, outlet adaptor covers 3-way
distilling adaptor
-roundbottom flask w/ sample 1/2 - 2/3 full
a. same level of surr. water
b. boiling chips
c. heated
-glass joints are well-fitted!
-vacuum adapter open to air
-rate of dripping: 2 drops distillate/sec
-DO NOT distill to dryness
E8: Relative Rates of Bromination

Steam Distillation
-2 round-bottom flasks
– Both with HEAT ON
– Flask 1: 1/2 full water (w/ pressure
– Flask 2: sample (closer to condenser,
w/ thermometer → mind the level)
– Connected thru steam glass tube
-UNSUBMERGED: thermometer, steam glass
-SUBMERGED: pressure regulator
-Condenser and receiving flask

E12: Carboxylic and Carboxylic Acid Derivatives

• Receiving flask w/ condenser on top
– Water in nearest the flask
– Flask half full
– Surrounded by water/oil bath (same
level as flask)
• Hot plate: ON