反应详情

温度

105 °C

1-(5-(Benzyloxy)-7-formylbenzo[d]thiazol-2-yl)-3-ethylurea (425 mg, 1.20 mmol), methoxylamine hydrochloride (105.2 mg, 1.26 mmol) and N,N′-diisopropylethylamine (0.77 g, 1.05 ml) were stirred in DMF degassed with N2. The reaction was purged with N2, sealed and heated to 105° C. for 18 h. LCMS after indicated complete consumption of starting material. The solvents were removed under reduced pressure and the resulting residue absorbed onto silica and purified by flash column chromatography eluting with 0 to 100% EtOAc in petroleum-ether to afford the product as a white solid 325 mg (70%) which was used directly in the next step.

1. customdegassed with N2
2. customThe reaction was purged with N2
3. customsealed
4. customconsumption of starting material
5. customThe solvents were removed under reduced pressure
6. customthe resulting residue absorbed onto silica
7. custompurified by flash column chromatography
8. washeluting with 0 to 100% EtOAc in petroleum-ether