반응 #45416

반응 방정식

3-bromo-4-chlorothieno[3,2-c]pyridine

NH4OH

→

desired product

수율 94.0%

3-bromothieno[3,2-c]pyridin-4-amine

수율 94.0%

용매

p-dioxane

반응 조건

후처리

1. 1
   기타prepared
2. 2
   농축The mixture was concentrated to half its original volume
3. 3
   workup.ADDITIONdiluted with water
4. 4
   추출extracted with ethyl acetate
5. 5
   세척The combined organic extracts were washed with brine
6. 6
   건조dried (MgSO4)
7. 7
   여과filtered
8. 8
   농축concentrated

실험 절차

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)+.

출처