تفاعل #75485

ord-606789d692104e22ac4861c45ccccd21

المتفاعلات

الكواشف

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ظروف التفاعل

درجة الحرارة
72.5°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe solvent was evaporated
  2. 2
    ترشيحThe resulting solid was filtered
  3. 3
    غسيلwashed with EtOAc/MeOH

الإجراء التجريبي

A mixture of 5-chloro-pentadione (5.12 g, 38 mmol) and thionicotinamide (5.25 g, 38 mmol) in MeOH (10 mL) was treated with pyridine (3 mL). The reaction mixture was heated at 70-75° C. for 5 h. The solvent was evaporated. The resulting solid was filtered and washed with EtOAc/MeOH to afford 4.33 g 5-acetyl-4-methyl-2-(3-pyridyl)-thiazol as a yellow solid, which was subjected to the next reaction without further purification. A mixture of this material (2.0 g) and N,N-dimethylformamide dimethyl acetal (4 mL) was heated at 80° C. for 22 h. The reaction mixture was concentrated and then triturated with EtOAc/PE. The precipitates were collected and washed with EtOAc/PE to afford the title compound (2.05 g, 75%) as a grey solid.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06699854B2uspto-grants-2004_03