تفاعل #45416
ord-e881c0334a2a48b98860a4e212b56dcb
معادلة التفاعل
الكواشف
لا شيء
المذيبات
ظروف التفاعل
درجة الحرارة
150°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.
المعالجة
- 1أخرىprepared
- 2تركيزThe mixture was concentrated to half its original volume
- 3workup.ADDITIONdiluted with water
- 4استخلاصextracted with ethyl acetate
- 5غسيلThe combined organic extracts were washed with brine
- 6تجفيفdried (MgSO4)
- 7ترشيحfiltered
- 8تركيزconcentrated
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)+.