Transition metal dichalcogenides (TMDCs) have received attention as atomically thin post‐silicon semiconducting materials. Tuning the carrier concentrations of the TMDCs is important, but their thin structure requires a non‐destructive modulation method. Recently, a surface‐charge transfer doping method was developed based on contacting molecules on TMDCs, and the method succeeded in achieving a large modulation of the electronic structures. The successful dopant is a neutral benzyl viologen (BV
0
); however, the problem remains of how to effectively prepare the BV
0
molecules. A reduction process with NaBH
4
in water has been proposed as a preparation method, but the NaBH
4
simultaneously reacts vigorously with the water. Here, a simple method is developed, in which the reaction vial is placed on a hotplate and a fragment of air‐stable metal is used instead of NaBH
4
to prepare the BV
0
dopant molecules. The prepared BV
0
molecules show a strong doping ability in terms of achieving a degenerate situation of a TMDC, MoS
2
. A key finding in this preparation method is that a convection flow in the vial effectively transports the produced BV
0
to a collection solvent. This method is simple and safe and facilitates the tuning of the optoelectronic properties of nanomaterials by the easily‐handled dopant molecules.