So the ratios are 100 ml D-H20 . Pour in 25 ml of high concentrate %60-75% nitric acid. Then, pour in 2 grams of sodium nitrite (catalyst) dilated with 5 mls D-H20 slowly. DON'T FREAK OUT NOR BREATH THE BROWN NITROUS FUMES COMING OFF ! Add 80 ml of benzyl alcohol. Then, reflux a low 75C-90C for 4 hours.
There will be some color changes , like a dark green.
Separate with a separatory funnel . Do a sodium bicarbonate (baking soda OTC) washing 1 - 2 times
*A color change to an orangish color and a change from bottom layer to a top layer may be noted *** KEEP WATCH AND MAKE NOTE OF ANY CHANGES **
Do a table salt brine wash
Do a water wash
Dry with anhydrous Magnesium Sulfate
Filter
Now distill the crude benzaldehyde at 179C-180C
*VACUUM DISTILLATION WILL LOWER THE NECESSARY DISTILLATION TEMPERATURE AND PREVENT CHEMICAL DECOMPOSITION BECAUSE OF HIGH HEAT AT REGULAR ATMOSPHERIC 760mmHg PRESSURE
Finish
**IT IS HIGHLY RECOMMENDED TO USE THIS FINISHED PRODUCT RIGHT AFTER IMMEDIATELY BECAUSE OF SUCH UNSTABLE DECOMPOSITION OF PURE RIGHT AFTER DISTILLED BENZALDEHYDE. Store properly.
Notes :
1) post RXN, there may not be a dark green color change but simply Orange ish
2) post RXN, the benzaldehyde will be on the bottom
3) smell of "cherry walnuts vanilla" will be noted
4) swim noticed 3/4 benzyl alcohol --oxidation to benzaldehyde references used a ~100 ml D-H20 to start with a small amount of concentration nitric acid
5) Another reference used 200ml D-H20 instead of 100 ml D-H20
Another reference used 30 ml concentration nitric acid and this reference used 50 grams concentrate nitric acid
*Sodium nitrite acts as a helpful catalyst*
Another reference used as low as 30-40 ml Benzyl alcohol this reference used 66 ml
Thank you
There will be some color changes , like a dark green.
Separate with a separatory funnel . Do a sodium bicarbonate (baking soda OTC) washing 1 - 2 times
*A color change to an orangish color and a change from bottom layer to a top layer may be noted *** KEEP WATCH AND MAKE NOTE OF ANY CHANGES **
Do a table salt brine wash
Do a water wash
Dry with anhydrous Magnesium Sulfate
Filter
Now distill the crude benzaldehyde at 179C-180C
*VACUUM DISTILLATION WILL LOWER THE NECESSARY DISTILLATION TEMPERATURE AND PREVENT CHEMICAL DECOMPOSITION BECAUSE OF HIGH HEAT AT REGULAR ATMOSPHERIC 760mmHg PRESSURE
Finish
**IT IS HIGHLY RECOMMENDED TO USE THIS FINISHED PRODUCT RIGHT AFTER IMMEDIATELY BECAUSE OF SUCH UNSTABLE DECOMPOSITION OF PURE RIGHT AFTER DISTILLED BENZALDEHYDE. Store properly.
Notes :
1) post RXN, there may not be a dark green color change but simply Orange ish
2) post RXN, the benzaldehyde will be on the bottom
3) smell of "cherry walnuts vanilla" will be noted
4) swim noticed 3/4 benzyl alcohol --oxidation to benzaldehyde references used a ~100 ml D-H20 to start with a small amount of concentration nitric acid
5) Another reference used 200ml D-H20 instead of 100 ml D-H20
Another reference used 30 ml concentration nitric acid and this reference used 50 grams concentrate nitric acid
*Sodium nitrite acts as a helpful catalyst*
Another reference used as low as 30-40 ml Benzyl alcohol this reference used 66 ml
Thank you
