I need help from experts: what equipment is required for this process?
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Triphenylphosphine, tert-butyl chloroacetate, and dichloromethane were added to the reactor in sequence, the temperature was raised to reflux, and the reaction was carried out at reflux for 2 hours. Cool, let stand for 20 h, then filter. The filter cake was washed with ether at 10°C, and the mother liquor and washing liquid were collected separately to yield a filter cake containing (tert-butoxycarbonylmethyl)triphenylphosphonium chloride (2) (71% purity). I wonder what equipment needs to be chosen for each processing step? Especially when the temperature is raised to the reflux point. Thank you
Should a shell-and-tube condenser be considered for heating and reflux?
Use a reactor with a jacket or an external coil; internal coils are not recommended. Based on experience, a reflux tower is necessary for reflux – a packed tower will suffice, along with a tubular condenser and a tank (which can allow overflow at a higher level), or forced reflux pumps can be used at a lower level; the reflux should flow into the reflux tower. Adding a centrifuge will do the trick.
Feed additives? It’s very simple.