hexylurea

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 6.0 g (0.1 mole) of urea and 11.1 g (0.11 mole) of n-hexylamine was heated at 130°-135° C. for 4 hours to form monohexylurea. Without isolation, the reaction mixture was cooled to 70° C., and 31.0 g (0.21 mole) of chloral was slowly added while the temperature was maintained below 80° C. using external cooling. The reaction mixture was vigorously stirred and heated at 80°-85° C. for 1 hour. On cooling 43.9 g of a viscous syrupy product was isolated. was heated at 130°-135° C. for 4 hours

Conditions: temp:0.00; pressure:0.00; stir:

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: 21.0 g of glyoxylic acid benzyl ester benzyl alcoholate and 10.0 g of N-hexylurea were refluxed in an 80% aqueous solution of acetic acid for 1.5 hours. After cooling, the reaction mixture was evaporated to dryness under reduced pressure. The obtained crude product was purified by column chromatography on silica gel (ethyl acetate:hexane=1:1) and was recrystallized from benzene to give 1.4 g of 5-hydroxy-1-hexylhydantoin (compound 12) in the form of colorless needle crystals. After cooling the reaction mixture was evaporated to dryness under reduced pressure The obtained crude product was purified by column chromatography on silica gel (ethyl acetate:hexane=1:1) was recrystallized from benzene

Conditions: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

Procedure: A mixture of 6.0 g (0.1 mole) of urea and 11.1 g (0.11 mole) of n-hexylamine was heated at 130°-135° C. for 4 hours to form monohexylurea. Without isolation, the reaction mixture was cooled to 70° C., and 31.0 g (0.21 mole) of chloral was slowly added while the temperature was maintained below 80° C. using external cooling. The reaction mixture was vigorously stirred and heated at 80°-85° C. for 1 hour. On cooling 43.9 g of a viscous syrupy product was isolated. was heated at 130°-135° C. for 4 hours