Question


U URUS, U JUU J 2. Fill in the reaction table below. Make sure you correctly calculate the molar amounts (mol.- eq.) of your

Synthesis of crude product.
1. Combine reagents (following either step A or B, depending on the benzaldehyde assigned to

you). It is best not to use a brand-new conical vial right out of the package, as the surface is not rough enough to help induce precipitation.

A. In a 5-mL conical vial, combine 0.15 g of 3-nitrobenzaldehyde (151.121 g/mol), 0.12 mL

of acetophenone (120.151 g/mol; d = 1.03 g/mL), and 0.80 mL of 95% ethanol.

OR

B. Pipette 0.13 mL of 4-anisaldehyde (136.150 g/mol) in a pre-weighed 5-mL conical vial, and record the mass. Then add 0.12 mL of acetophenone (120.151 g/mol; d = 1.03 g/mL) and 0.80 mL of 95% ethanol.

2. Stir the solution until any solids are dissolved. Gentle heat (< 60 ° C) from a water bath may be needed.

  1. Add 0.10 mL of 15 M NaOH, and stir until a solid forms. Precipitation can take 5 – 15 min. If after 15 min precipitate does not form, try scratching the inner surface of the conical vial with a glass rod. If precipitation is still not occurring, then heat gently for 10 – 15 min.

  2. Add 2 mL of ice water to the precipitate in the conical vial, stir, then transfer this mixture to a beaker containing another 3 mL of ice water. (This step ultimately adding 5 mL of ice water to the precipitate—2 mL then 3 mL).

  3. Filter the chalcone product using a Hirsch funnel (with pre-weighed filter paper) and vacuum filtration. Rinse the beaker and product with two 1-mL portions of ice-cold DI water. Transfer filter paper and precipitate to a pre-weighed watch glass.

    **At this point, the product will either be dried for 10 min, recrystallized (optional), or dried until the next lab period.**

Recrystallization (optional).

  1. Either microscale or Craig tube approach may be used.

  2. Add hot solvent* dropwise until the chalcone just dissolves. For microscale, recrystallize all of the product.
    A. *3-nitrochalcone. Solvent is hot methanol. For Craig tube, use 0.025 g chalcone and 1 mL solvent.

    OR
    B. *4-methoxychalcone. Solvent is hot 95% ethanol. For Craig tube, use 0.075 g chalcone and 0.3 mL solvent.

3. Cool slowly to room temperature. Then place on ice to complete the precipitation, and collect the recrystallized product.

The question I am asking is how to do the moles and mmoles? Please help, I already figured out the density of the product.

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Answer #1

PAGE No Moles Gwen mass (m Molecular weight (HW) i) 3- Nitrobenzaldehyde - M = 0.15 9 MW = 151-12 moles = = 0.00099 moles 0.1

d = 1.039 mL M = 120.151 as_m m 1 .03X 0:12 - = 0.1236 moles = 0.1236 = 0.00102 moles 120.15 = 1.02 X 10-3 moles = 1:02 mmole

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