Mohammed Salam Unit 14: LA D
Investigate organic chemistry reactions in order to gain skills in preparative organic chemistry.
Making designer chemicals.
Preparation of 1 – bromobutane:
1. 30cm3 of water should be placed in the 250cm3 round bottomed flask. Add 35 g of
powdered sodium bromide and 25cm3 of butan – 1 – ol into the round bottomed flask.
2. Tap funnel should be fitted via stillhead.
3. 25 cm3 of concentrated of sulphuric acid should be placed in the tap funnel. Allow the acid
to drop wise into the flask. Ensure that the contents are well shaken and cooled in an ice
water bath.
4. Replace the tap funnel and stillhead with a reflux condenser once the addition is completed.
Allow the mixture to gently boil over a sand bath for approximately 45 minutes. Shake the
flask gently throughout the procedure.
5. Distil the crude 1 bromobutane, this should be done after removing the reflux condenser
and when the apparatus is rearranged for distillation.
6. The distillate should be gently shaked with water in a separating funnel. Run off the lower
layer of 1 bromobutane omit the aqueous layer formed by this process.
7. The 1 bromobutane should be added back to the funnel, add approximately half of the
volume of 1 bromobutane of concentrated hydrochloric acid then shake. Discard the lower
layer of the acid.
8. Dilute sodium carbonate solution should be added when cautiously shaking the 1
bromobutane, release the pressure at intervals.
9. Add some granular anhydrous calcium chloride into the lower layer of 1 bromobutane. The
mixture should be swirled until the solution becomes transparent.
10. The 1 bromobutane should be filtered into the clean dry flask and distil the 1 bromobutane.
Collect the fraction boiling between 99 to 102 degrees.
1
, Mohammed Salam Unit 14: LA D
Substance Hazard Precaution
Sulphuric acid Corrosive Use the lowest concentration as
Can cause skin burns if possible in the practical.
contact on skin Wear the appropriate PPE
equipment like gloves and
goggles.
1 – bromobutane Flammable Avoid from contacting with
naked flames
Sodium bromide Sodium bromide is Wear goggles and gloves.
hazardous in case of eye Move to well ventilated area.
contact, ingestion, and
inhalation. It is slightly
hazardous in case of skin
contact
Hydrochloric acid Corrosive Wear appropriate PPE like
Can cause burns to skin gloves when handling the acid.
Use the lowest concentration as
possible.
Anhydrous calcium chloride Anhydrous calcium chloride Wear appropriate PPE
is a dangerous chemical that equipment like goggles and
can cause severe skin gloves.
irritation and burns to the Move to well ventilated area if
eyes, respiratory tract, and symptoms begins to occur when
skin. handling the substance.
Sodium carbonate Irritant – can affect lungs, Wear appropriate PPE
skin and eyes. equipments like gloves and
goggles.
Move to well ventilated site if
symptoms begins to occur when
handling the substance.
Preparation of ethanoic acid from ethanol:
2
Investigate organic chemistry reactions in order to gain skills in preparative organic chemistry.
Making designer chemicals.
Preparation of 1 – bromobutane:
1. 30cm3 of water should be placed in the 250cm3 round bottomed flask. Add 35 g of
powdered sodium bromide and 25cm3 of butan – 1 – ol into the round bottomed flask.
2. Tap funnel should be fitted via stillhead.
3. 25 cm3 of concentrated of sulphuric acid should be placed in the tap funnel. Allow the acid
to drop wise into the flask. Ensure that the contents are well shaken and cooled in an ice
water bath.
4. Replace the tap funnel and stillhead with a reflux condenser once the addition is completed.
Allow the mixture to gently boil over a sand bath for approximately 45 minutes. Shake the
flask gently throughout the procedure.
5. Distil the crude 1 bromobutane, this should be done after removing the reflux condenser
and when the apparatus is rearranged for distillation.
6. The distillate should be gently shaked with water in a separating funnel. Run off the lower
layer of 1 bromobutane omit the aqueous layer formed by this process.
7. The 1 bromobutane should be added back to the funnel, add approximately half of the
volume of 1 bromobutane of concentrated hydrochloric acid then shake. Discard the lower
layer of the acid.
8. Dilute sodium carbonate solution should be added when cautiously shaking the 1
bromobutane, release the pressure at intervals.
9. Add some granular anhydrous calcium chloride into the lower layer of 1 bromobutane. The
mixture should be swirled until the solution becomes transparent.
10. The 1 bromobutane should be filtered into the clean dry flask and distil the 1 bromobutane.
Collect the fraction boiling between 99 to 102 degrees.
1
, Mohammed Salam Unit 14: LA D
Substance Hazard Precaution
Sulphuric acid Corrosive Use the lowest concentration as
Can cause skin burns if possible in the practical.
contact on skin Wear the appropriate PPE
equipment like gloves and
goggles.
1 – bromobutane Flammable Avoid from contacting with
naked flames
Sodium bromide Sodium bromide is Wear goggles and gloves.
hazardous in case of eye Move to well ventilated area.
contact, ingestion, and
inhalation. It is slightly
hazardous in case of skin
contact
Hydrochloric acid Corrosive Wear appropriate PPE like
Can cause burns to skin gloves when handling the acid.
Use the lowest concentration as
possible.
Anhydrous calcium chloride Anhydrous calcium chloride Wear appropriate PPE
is a dangerous chemical that equipment like goggles and
can cause severe skin gloves.
irritation and burns to the Move to well ventilated area if
eyes, respiratory tract, and symptoms begins to occur when
skin. handling the substance.
Sodium carbonate Irritant – can affect lungs, Wear appropriate PPE
skin and eyes. equipments like gloves and
goggles.
Move to well ventilated site if
symptoms begins to occur when
handling the substance.
Preparation of ethanoic acid from ethanol:
2
