synthesis Flashcards

1
Q

fingerprint region

A

below 1500

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2
Q

rough area of C-H peak

A

3000

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3
Q

molecular ion peak

A

highest peak, on right hand side of mass spectrum = molecular mass of compound/substance

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4
Q

amount of bond bend/strectch depends on: (2)

A
  • mass of atoms (heavier = vibrate more)

- strength of bonds (stronger = vibrate more/faster)

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5
Q

SHC eq.

A

q (heat energy given out) = mcΔT

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6
Q

enthalpy change (per mole) eq.

A

= -q / number of moles reacting

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7
Q

what do you need for heating under reflux? (5)

A
  • pear shaped flask
  • condenser
  • rubber tubing
  • stand and clamp
  • heat source
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8
Q

what do you need for distillation? (9)

A
  • pear shaped flask
  • condenser
  • rubber tubing
  • heat source
  • stand and clamp
  • screw cap adaptor
  • receiver adapter
  • still heat
  • thermometer
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9
Q

how do you separate an organic product (liquid)

A
  • pour mix into funnel
  • place stopper on and invert
  • add water to see which layer increases in volume = aq layer
  • place conical flask under and open tap, until lower layer is gone
  • add Na2CO3, add stopper and invert, open tap and allow gas to escape - removes acid impurities
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10
Q

how do you purify a (separated) organic product (liquid) – [drying]
- agent typically used

A
  • add drying agent using spatula (CaSO4) and swirl
  • place stopper to prevent evaporation and leave for 10
  • if solid is stuck together there is still liquid - add more drying agent and repeat
  • continue adding until solid is dispersed like a fine powder
  • decant liquid into another flask
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11
Q

how do you separate a solid from liquid mixture?

A
  • connect pressure tubing to vacuum outlet and attach other end to Buchner flask
  • fit funnel to flask, ensuring tight fit by using a bung
  • switch vacuum on
  • check for suction by placing hand over funnel
  • put filter paper in funnel - wet with solvent used in mixture
  • slowly add mixture into centre of funnel
  • rinse beaker with solvent so that all crystals collect in funnel
  • rinse crystals in funnel with more solvent and leave for a few mins to start to dry
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12
Q

what do you need for filtration under reduced pressure?

A
  • Buchner flask
  • Buchner funnel
  • pressure tubing
  • filter paper
  • access to vacuum pump to filter
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13
Q

method for recrystallisation

A
  • pour solvent into conical flask
  • if flammable heat with water bath, if not use bunsen
  • add sample to second beaker
  • slowly add hot solvent to sample until sample just dissolves
  • once dissolved, allow to cool - crystals should form
  • when no more forms filter under reduced pressure to get solid
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14
Q

melting range

A

difference between temperatures at which sample starts to melt and melting is complete

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15
Q

if sample contains impurities…

….

A

range is wider

melting point is lower

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16
Q

preparation for melting point determination

A
  • ensure sample completely dry
  • take capillary tube and heat end in bunsen until is sealed
  • allow to cool and then add sample until about 3mm deep
17
Q

2 methods of melting point determination

A

1) electrically heated melting point apparatus

2) oil bath/Theile tube method

18
Q

how does electrically heated melting point apparatus method work?

A
  • place capillary tube w sample in sample hole
  • place thermometer in thermometer hole
  • use rapid heat setting - observe through magifying window
  • once solid has started to melt, stop and record temp
  • repeat on low setting and observe = more accurate
19
Q

how does Theile tube/oil bath method work?

A
  • set up T. tube or oil bath
  • attach capillary tube to thermometer using elastic band
  • insert thermometer through hole in cork (/clamp it if using oil bath)
  • use micrometer to slowly heat - record temp when starts to heat
  • repeat for accuracy
20
Q

further purification after distillation

A
  • pour solution into separating funnel and shake
  • separate layers by tapping off
  • add small amount of CaSO4 to organic layer in dry conical flask
  • redistill organic layer
  • collect fraction distilling at 150-156C