تفاعل #1726704

ord-d7ddcf975d934cd196baeb7fb4c03fd9

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةheated
  2. 2
    درجة الحرارةto reflux for 3.5 hr
  3. 3
    تركيزThe cooled mixture was concentrated in vacuo
  4. 4
    أخرىpartitioned between dichloromethane and saturated aqueous sodium bicarbonate
  5. 5
    غسيلThe organic phase was washed with brine
  6. 6
    تجفيفdried over sodium sulfate
  7. 7
    ترشيحfiltered
  8. 8
    تركيزconcentrated in vacuo

الإجراء التجريبي

α-Bromophenylacetonitrile (1.08 g, 5.48 mmol) in ethanol (10 ml) was treated with N-acetylthiourea (649 mg, 5.49 mmol) at ambient temperature for 4 hr, and then heated to reflux for 3.5 hr. The cooled mixture was concentrated in vacuo and then partitioned between dichloromethane and saturated aqueous sodium bicarbonate. The organic phase was washed with brine, dried over sodium sulfate, filtered and concentrated in vacuo. Flash chromatography on silica gel (ethyl acetate/hexanes) yielded 2-(acetylamino)-4-amino-5-phenylthiazole (295 mg, 23%).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08110568B2uspto-grants-2012_02