반응 #799258

반응 방정식

8-methylpyrazolo[1,5-c]thieno[2,3-e]pyrimidine

N-bromosuccinimide

→

desired product

9-Bromo-8-methylpyrazolo[1,5-c]thieno[2,3-e]pyrimidine

용매

methylene chloride

반응 조건

후처리

1. 1
   농축the reaction solution was concentrated
2. 2
   기타the resultant residue was purified with flash chromatography (
3. 3
   세척eluting with a gradient of 0-20% ethyl acetate in hexanes)

실험 절차

To a solution of 8-methylpyrazolo[1,5-c]thieno[2,3-e]pyrimidine (1.01 g, 5.34 mmol) in methylene chloride (30 mL) was added N-bromosuccinimide (0.959 g, 5.39 mmol). After stirring for 1 h, the reaction solution was concentrated, and the resultant residue was purified with flash chromatography (eluting with a gradient of 0-20% ethyl acetate in hexanes) to give the desired product as whited solid. 1H NMR (300 MHz, CD3OD) δ 9.11 (1H, s), 7.94 (1H, d, J=5.3 Hz), 7.52 (1H, d, J=5.3 Hz), 2.48 (3H, s) ppm. LCMS calculated for C9H7BrN3S (M+H)+: m/z=268.0. Found: 267.9.

출처