[Polly Murs]

so I have been trying to adapt a published method which uses benzyl alcohol.
I can get the benzyl alcohol to reflux (with the precursor dissolved), but then I try adding in another (higher boiling) solvent and it's now stuck on 160C.

I've done this reaction blank and the solvent mixture refluxed at around 245-250C... so why is it misbehaving now?

edit: 1g precursor + 20ml benzyl alcohol

after 2h I added in 30 mL of the other solvent (I'd prefer not to say what it is)

[kriggy]

So your reaction refluxed in benzyl alcohol at 160. The mixture of solvents without any reagents refluxed at 250?

[Polly Murs]

I do the reaction as standard in benzyl alcohol and bring it to reflux (205C). the oil bath is maxed out at 250C.

After 2h at reflux, I introduce the new solvent. There's a sharp drop to 160C, and it never really goes beyond this.
(Yet the blank that I ran (no precursor, just solvents) went to reflux at 250C)

[Polly Murs]

anyone?

every now and then the reaction mixture bumps. the pressure blew the thermometer pocket out at one point.

the total volume is 50 mL, in a 100 mL flask.

edit: I think I'm generating some side products during the nanoparticle synthesis. the precursor is iron(III)acetylacetonate