反应详情

A solution of 23.00 g (91.26 mmol) of methyl 3-amino-5-nitrobenzo[b]thiophene-2-carboxylate (J. Hetero. Chem, 34(4), 1163 (1997)) in 100 mL of 1-methyl-2-pyrrolidinone and 30 mL of 1-methylpiperazine is heated at 180° C. for 2 hours. The reaction is cooled to room temperature and poured into water. The resultant solid is collected by filtration and washed with water. The solid is dissolved in a mixture of ethyl acetate and diethyl ether and the solution is washed with water twice. The organic layer is dried over magnesium sulfate, filtered and concentrated in vacuo. Diethyl ether and hexane are added to the residue and the dark red solid is collected by filtration to provide 11.17 g (63%), mp 155–158° C.

1. filtrationThe resultant solid is collected by filtration
2. washwashed with water
3. dissolutionThe solid is dissolved in a mixture of ethyl acetate and diethyl ether
4. washthe solution is washed with water twice
5. dry with materialThe organic layer is dried over magnesium sulfate
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. additionDiethyl ether and hexane are added to the residue
9. filtrationthe dark red solid is collected by filtration
10. customto provide 11.17 g (63%), mp 155–158° C.