Part I
1) Dissolve 0.5 g naphthalene and 0.5 g in 20 mL of methylene chloride and transfer to the separating funnel.
Note that separating funnel will be checked before using the
2) Add 10 mL of 5% NaOH in a separatory funnel. Shake and reduce the pressure for three times. Wait until the solution separate into two layers.
3) Drain off the lower layer.
4) Pour the upper layer out of the top into another container.
5) Pour the lower layer into the same separatory funnel.
6) Repeat steps 2-5 for two times. Please note that the after you finished step 6, you will get 30 mL of the upper layer.
7) Dry the lower layer by added Na2SO4 anhydrous.
8) Filter (the beaker should be absolutely dried), evaporate (in water bath), collect your sample and determine mp.
9) Pour the upper layer, 30 mL, (from step 6) into separatory funnel.
10) Acidify with 20% HCl. (In this step, the solution will change from base (NaOH) to acid (HCl) and you will see white solid is precipitated).
11) Add 10 mL of CH2Cl2 in a separatory funnel. Shake and reduce pressure for three times. Wait until the solution separate into two layers.
12) Drain off the lower layer and keep it.
13) Repeat steps 11 and 12 for two times. At this step, you will get 30 mL of lower layer.
14) Repeat steps 7 and 8.
Part I
1) Dissolve 0.5 g naphthalene and 0.5 g in 20 mL of methylene chloride and transfer to the separating funnel.
Note that separating funnel will be checked before using the
2) Add 10 mL of 5% NaOH in a separatory funnel. Shake and reduce the pressure for three times. Wait until the solution separate into two layers.
3) Drain off the lower layer.
4) Pour the upper layer out of the top into another container.
5) Pour the lower layer into the same separatory funnel.
6) Repeat steps 2-5 for two times. Please note that the after you finished step 6, you will get 30 mL of the upper layer.
7) Dry the lower layer by added Na2SO4 anhydrous.
8) Filter (the beaker should be absolutely dried), evaporate (in water bath), collect your sample and determine mp.
9) Pour the upper layer, 30 mL, (from step 6) into separatory funnel.
10) Acidify with 20% HCl. (In this step, the solution will change from base (NaOH) to acid (HCl) and you will see white solid is precipitated).
11) Add 10 mL of CH2Cl2 in a separatory funnel. Shake and reduce pressure for three times. Wait until the solution separate into two layers.
12) Drain off the lower layer and keep it.
13) Repeat steps 11 and 12 for two times. At this step, you will get 30 mL of lower layer.
14) Repeat steps 7 and 8.
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