Note: The following story is a work of fiction.
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A researcher recently attempted to make 2C-B for the third time. These are the notes from his lab notebook:
2:30a A 250 mL flask is weighed with a paper collar and found to weigh 113.68 g.
2:37a A piece of paper was weighed and found to weigh 1.37 g. A quantity of the presumed 2C-H HCl in the form of fine white needles was weighed on the paper. Weight (w/ paper): 29.35 g. Weight (w/o paper): 29.35 - 1.37 = 27.98 g.
2:44a The 2C-H was placed in a 500 mL beaker. 50.00 mL H2O was added. Most of the 2C-H dissolved.
2:57a An additional 10 mL was added. This appeared to dissolve all of the 2C-H. The solution was placed in a 250 mL separation funnel.
3:04a 40 mL H2O was placed in a beaker. 12.5 g NaOH was added. The hot solution was cooled in the refrigerator.
3:21a The NaOH solution was added to the funnel. The solution became cloudy and separated into two layers, with the 2C-H freebase on top.
Note: The researcher was surprised to learn that 2C-H freebase floated on water after having read
https://www.thevespiary.org/rhodium/Rhodium/chemistry/2cb.large-scale.bromination.html
.
3:27a The water layer was drained. The 2C-H was placed in a 250 mL round-bottom flask that had been previously weighed. The weight was taken: 143.46 g
3:34a Since the calculated weight of the freebase was 29.78g, it was assumed that some water had gotten into the oil. 23 g was used as the weight instead.
3:38a 40*23/24.8 = 37 mL of GAA was added. Not liking the smell of GAA, I attached a reflux column. The mixture was placed under stirring.
3:51a Time for the scary part. 37 mL of GAA was placed in a 50 mL Erlenmeyer flask. 6.5 mL Br2 was added to it, and the solutions were combined. The reaction mixture took on a black color.
Note: This was done without a fume hood in a dorm room. That was crazy!
4:12a Disaster! The flask fell on the ground and broke. 2C-B congeals on my floor. I scape up the dark brown sludge and place it in a Buchner funnel, wash it with 2x3 mL GAA (improving the color considerably).
~4:30a Dissolved some of the scrapings in H2O. Filtered. Placed the solution in a separation funnel. Added NaOH solution to make the solution strongly basic. Noted that a black oil settled out. Added 10 mL DCM. Mixed. Allowed to settle.
Note: 2C-B freebase is heavier than H2O.
~5:00a Went to get razor blades at the grocery store for further scraping. Noted a strong scent of bromine in the neighborhood.
~5:20a Removed DCM layer. Added an additional 10 mL. Mixed. Allowed to settle. Drained DCM and added to other DCM.
6:04a Stripped DCM under vacuum.
6:54a Stripping finished. About 2mL of a dark oil remains. Took a nap.
5:30p Placed the oil in a pre-weighed GAA/H2O mix w/ 3 mL H2O and 1 mL GAA. An additional 1 mL H2O was added. Weight: 46.70 g w/ beaker. Weight w/ freebase: 50.93 g. Weight of freebase: 4.23 g. An additional 3.4 mL H2O was added. Not quite everything dissolved, so the beaker was heated slightly. 3.00 mL 37% HCl was added. Crystals formed quickly. The mixture was filtered, washed with 3x2 mL H2O and washed with 2x2 mL DCM. DCM appears to dissolve 2C-B HCl slightly. The substance remained a tan color.
6:45p The glistening tan 2C-B HCl crystals were weighed and found to be 1.67 g. 10 mg were placed in a capsule, which was eaten.
2:29a I experienced no nausea after eating the pill, which was eaten immediately before a full meal. Within an hour, I noticed that I was tripping quite hard, but that I still had very good clarity of thought and my decision-making processes seemed to be intact. I think I peaked at around 10:00. The experience was extremely pleasant. Unfortunately, though this product is quite pure, it is not pure enough. A full distillation of the freebase is in order, and DCM cannot be substituted for ether in the final washes. I have further floor scrapings that will hopefully contain more product that can be treated appropriately.
Additional testing of the product will be done in the next few days. My skills are rapidly improving.
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Oxygen69