Table 2.

Screening of the liquid additives for Biltz synthesis to Phenytoin (4) by RAM.^a)

Entry	Influence of	Liquid additive	η [μL mg−1]	Time [min.]	Yield [%]b)
1	LAG solvent	H2O	0.5	180	14
2		Glycerol	0.5	180	n.r.c)
3		EtOH	0.5	180	67
4	η value	EtOH	0.05	90	41
5		EtOH	0.1	90	24
6		EtOH	0.25	90	39
7d)		EtOH	0.5	90	81
8		EtOH	0.75	90	99
9	Reaction time	EtOH	0.75	60	99
10		EtOH	0.75	20	98 (79%)e)
11		EtOH	0.75	10	26

^a)Reaction was conducted in a 10 mL screw cap glass vial. Reaction conditions: benzil (5.35 mmol, 1.0 equiv.), urea (5.35 mmol, 1.0 equiv.) and KOH (10.7 mmol, 2.0 equiv.) were accelerated at 90 g during 180 min, except when otherwise specified;

^b)Yields were calculated by quantitative GC‐MS using a linear calibration curve obtained by using commercial phenytoin, except when otherwise specified (see Supporting Information for more details);

^c)n.r. = No reaction;

^d)Pre‐grinded KOH was used;

^e)Isolated yield.