Hi it would be appreciated if I can have constructive comments on my synthesis path. If you can reccomed any practical changes or if anything looks off please be prepared to explain why you would change something.
**Preparation:**
1. **NaOH Solution Preparation:** Dissolve 90g of NaOH in 100ml of water. Freeze this mixture overnight.
**Synthesis Process:**
**Phase 1: in reactor using over head stirrer**
- Add, 100g of 2b3c and dissolve in 300ml of ethyl acetate, stirring rigorously 2 minutes.
- Add the pre-prepared, ice cold NaOH mixture and stir for an additional 2 minutes.
**Phase 2: Exothermic Reaction**
- Gradually introduce 150g of MA HCl, initiating an exothermic reaction that increases the temperature to approximately 30°C. Continue stirring throughout this phase.
**Phase 3: **
- Maintain stirring while applying heat to keep a constant temperature of about 37°C for 2 hours.
**Phase 4: Impurity Removal** reactor/ separation funnel
- Add, 300ml of chilled deionized water and 2-3g of baking soda to reactor. Stir for 1 minute rigorously, then drain to remove the "dirty" water along with soluble impurities. Add to separating funnel and remove the water layer. Repeat the washing process one or two more times as necessary, to attain a oil without a very strong solvent smell.
Phase 5 **Drying Purification:**
Pour washed oil into a beaker and add anhydrous sodium sulfate to the beaker as a drying agent to absorb any water. Keep adding the sodium untill it no longer clumps and u see free flowing crystals.
- Once there is no more water in the oil, use vacuum filtration to remove the anhydrous sodium sulfate and any remaining particulate matter. Transfer back into a clean dry beaker.
phase 6 **Acidification:**
- Prepare a mixture of 100ml acetone and 100ml HCl in a drip funnel
- Place beaker with tour now dry oil in an ice bath to keep the temperature around 10°C.
- Slowly add the acid mixture to the oil until reaching a pH of 6, monitoring for precipitation.
- Store the beaker with your 3cmc powder in the freezer overnight.
**Final Wash:**
- Wash the impurities off your powder with cold acetone the next day, we are aiming for a very powder devoid of solvent odors
**Preparation:**
1. **NaOH Solution Preparation:** Dissolve 90g of NaOH in 100ml of water. Freeze this mixture overnight.
**Synthesis Process:**
**Phase 1: in reactor using over head stirrer**
- Add, 100g of 2b3c and dissolve in 300ml of ethyl acetate, stirring rigorously 2 minutes.
- Add the pre-prepared, ice cold NaOH mixture and stir for an additional 2 minutes.
**Phase 2: Exothermic Reaction**
- Gradually introduce 150g of MA HCl, initiating an exothermic reaction that increases the temperature to approximately 30°C. Continue stirring throughout this phase.
**Phase 3: **
- Maintain stirring while applying heat to keep a constant temperature of about 37°C for 2 hours.
**Phase 4: Impurity Removal** reactor/ separation funnel
- Add, 300ml of chilled deionized water and 2-3g of baking soda to reactor. Stir for 1 minute rigorously, then drain to remove the "dirty" water along with soluble impurities. Add to separating funnel and remove the water layer. Repeat the washing process one or two more times as necessary, to attain a oil without a very strong solvent smell.
Phase 5 **Drying Purification:**
Pour washed oil into a beaker and add anhydrous sodium sulfate to the beaker as a drying agent to absorb any water. Keep adding the sodium untill it no longer clumps and u see free flowing crystals.
- Once there is no more water in the oil, use vacuum filtration to remove the anhydrous sodium sulfate and any remaining particulate matter. Transfer back into a clean dry beaker.
phase 6 **Acidification:**
- Prepare a mixture of 100ml acetone and 100ml HCl in a drip funnel
- Place beaker with tour now dry oil in an ice bath to keep the temperature around 10°C.
- Slowly add the acid mixture to the oil until reaching a pH of 6, monitoring for precipitation.
- Store the beaker with your 3cmc powder in the freezer overnight.
**Final Wash:**
- Wash the impurities off your powder with cold acetone the next day, we are aiming for a very powder devoid of solvent odors
