Reaction #2062754
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04268510
Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: 2-Amino-3-methylbenzyl alcohol (1.7 g.) and anhydrous chloral (2.4 ml.) were mixed for 10 minutes with external ice-cooling, and the mixture was left to stand for 1/2 hour. The mixture was then chromatographed on silica, and elution with diethyl ether/petroleum ether (b.p. 60°-80° C.), 7:3 by volume, gave 1,2-dihydro-8-methyl-2-trichloromethyl-4H-benzo[d]-[1,3]-oxazine, which was crystallised from aqueous ethanol, m.p. 69°-70° C. cooling the mixture was left The mixture was then chromatographed on silica, and elution with diethyl ether/petroleum ether (b.p. 60°-80° C.), 7:3 by volume
Source ID: ord-4d45462cfba040a9ad2f6abb6ba42fec