Preparative Scale Synthesis

The method described in Subheading 3.1. can be easily adjusted to a preparative scale by increasing the reaction volume. The flowchart in Fig. 1 is still valid except for the separation and sampling steps. The composition of the reaction mixture should be optimized prior to scaling up the synthesis. The reaction mixture can be prepared manually or with a laboratory mixer (see step 5). When carrying the synthesis, the reaction mixture should be mixed at regular time intervals (e.g., 1 h, and preferably continuously, to facilitate mass transfer.

Fig. 1. Flowchart of solid-to-solid synthesis on a laboratory scale.
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