تفاعل #45416

ord-e881c0334a2a48b98860a4e212b56dcb

الكواشف

لا شيء

المذيبات

ظروف التفاعل

درجة الحرارة
150°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىprepared
  2. 2
    تركيزThe mixture was concentrated to half its original volume
  3. 3
    workup.ADDITIONdiluted with water
  4. 4
    استخلاصextracted with ethyl acetate
  5. 5
    غسيلThe combined organic extracts were washed with brine
  6. 6
    تجفيفdried (MgSO4)
  7. 7
    ترشيحfiltered
  8. 8
    تركيزconcentrated

الإجراء التجريبي

A mixture of 3-bromo-4-chlorothieno[3,2-c]pyridine (prepared according to the procedure described in Bull. Soc. Chim. Belges 1970, 79, 407-414, 3 g, 12 mmol), concentrated aqueous NH4OH (100 mL), and p-dioxane (100 mL) was sealed in a stainless steel, high-pressure reactor and stirred for 18 hours at 150° C. The mixture was concentrated to half its original volume, diluted with water, and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried (MgSO4), filtered, and concentrated to provide 2.6 g (94%) of the desired product. 1H NMR (DMSO-d6, 400MHz) δ 7.83 (d, 1H), 7.77 (s, 1H), 7.26 (d, 1H), 6.48 (br s, 2H); MS m/e 229 (M+H)+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07737160B2uspto-grants-2010_06