This stuff doesnt dry very easily and im not going to bother with recrystralisation at this point. I attempted a MP test though of this unpurified substance and its something like 67-72c. It seemed to decompose though, losing some mass and becoming yellow.
After vac filtration the weight was around 40g, after some drying time it came down to 25g, but also taking on a light yellow colour. A day later and its still damp and 25g.
It will used as is in a rearrangement.
Edit: FYI, 2.83g of CYA was filtered, a bit above the molar equivalent of TCCA that went in. The extra weight could possibly be some N-Chloroamide that had precipitated, I dont know - the CYA was dried to a crisp so I dont think it was moisture.
After vac filtration the weight was around 40g, after some drying time it came down to 25g, but also taking on a light yellow colour. A day later and its still damp and 25g.
It will used as is in a rearrangement.
Edit: FYI, 2.83g of CYA was filtered, a bit above the molar equivalent of TCCA that went in. The extra weight could possibly be some N-Chloroamide that had precipitated, I dont know - the CYA was dried to a crisp so I dont think it was moisture.