반응 #166192

반응 방정식

2-bromo-4-fluoro-3-formyl-benzoic acid tert-butyl ester

hydrazine hydrate

→

title compound

수율 100.0%

4-Bromo-1H-indazole-5-carboxylic acid tert-butyl ester

수율 100.0%

용매

DME

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   기타the products were partitioned between ethyl acetate and water
3. 3
   추출the aqueous layer extracted with ethyl acetate
4. 4
   건조the combined organic extracts dried (Na2SO4)
5. 5
   여과filtered
6. 6
   농축concentrated in vacuo

실험 절차

A bi-phasic solution of 2-bromo-4-fluoro-3-formyl-benzoic acid tert-butyl ester (4.25 g, 14 mmol), DME (25 mL) and hydrazine hydrate (15 mL) was heated at 90° C. for 1 hour. After cooling, the products were partitioned between ethyl acetate and water, the aqueous layer extracted with ethyl acetate and the combined organic extracts dried (Na2SO4), filtered and concentrated in vacuo to give the title compound as a tan solid (4.1 g, 100%). LCMS (method B) RT=3.63 min, [M+CH3CN+H]+=338/340, [M−H]−=295/297.

출처