تفاعل #49959

ord-de9bab9b5e424189ac8c17363b982488

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةunder reflux for 2 hours
  2. 2
    ترشيحThe resulting crystals were collected by filtration
  3. 3
    غسيلwashed with cold acetone
  4. 4
    أخرىdried under reduced pressure
  5. 5
    workup.ADDITIONThe crystals were added to 50 ml of 30% methylamine-methanol
  6. 6
    workup.STIRRINGthe mixture was stirred at room temperature overnight
  7. 7
    تركيزThe reaction mixture was concentrated to dryness under reduced pressure
  8. 8
    غسيلthe residue was washed with ethanol-ethyl acetate
  9. 9
    أخرىdried under reduced pressure

الإجراء التجريبي

To 50 ml of acetone were added 2.46 g of o-anisidine and 3.75 g of benzoyl isothiocyanate, and the mixture is stirred under reflux for 2 hours and, then, allowed to stand overnight in a refrigerator at 5° C. The resulting crystals were collected by filtration, washed with cold acetone and dried under reduced pressure. The crystals were added to 50 ml of 30% methylamine-methanol and the mixture was stirred at room temperature overnight. The reaction mixture was concentrated to dryness under reduced pressure, and the residue was washed with ethanol-ethyl acetate and dried under reduced pressure. The procedure provided 2.08 g of N-(o-methoxyphenyl)thiourea.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05424431uspto-grants-1995_06