反应详情

A mixture of ethyl 2-[1-(methoxymethyl)-7-nitro-1H-indol-2-yl]-1,3-thiazole-5-carboxylate (2.44 g), iron(III) chloride hexahydrate (92 mg), activated carbon (1.0 g), tetrahydrofuran (10 mL) and ethanol (5 mL) was heated under reflux for 20 min. To the reaction mixture was added hydrazine monohydrate (2.05 g) over 15 min while heating under reflux. The reaction mixture was heated under reflux for 5 hr, filtrated, and the filtrate was concentrated. The residue was dissolved in ethyl acetate, washed with saturated brine, dried (MgSO4), and concentrated. Isopropyl ether was added to the obtained residue. The resulting crystals were collected by filtration, washed with isopropyl ether, and dried to give the title compound (2.18 g, yield 97%) as yellow crystals. melting point 188-190° C.

1. temperaturewas heated
2. temperatureunder reflux for 20 min
3. temperaturewhile heating
4. temperatureunder reflux
5. temperatureThe reaction mixture was heated
6. temperatureunder reflux for 5 hr
7. filtrationfiltrated
8. concentrationthe filtrate was concentrated
9. dissolutionThe residue was dissolved in ethyl acetate
10. washwashed with saturated brine
11. dry with materialdried (MgSO4)
12. concentrationconcentrated
13. additionIsopropyl ether was added to the obtained residue
14. filtrationThe resulting crystals were collected by filtration
15. washwashed with isopropyl ether
16. customdried