反应详情

温度

110 °C

A mixture of methyl 3-amino-5-bromothiophene-2-carboxylate (200 mg) produced in Example 1, step C, morpholine-4-carbonitrile (0.17 mL) and 4M hydrochloric acid/cyclopentylmethylether solution (3.0 mL) was stirred at 110° C. for 4 hr. The reaction system was concentrated under reduced pressure, and saturated aqueous sodium hydrogen carbonate was added to the residue. The precipitate was collected by filtration and washed with water. The obtained pale-brown solid was washed with a mixed solvent of ethyl acetate/hexane (1:1) to give the title compound (144 mg) as a pale-yellow solid.

1. concentrationThe reaction system was concentrated under reduced pressure, and saturated aqueous sodium hydrogen carbonate
2. additionwas added to the residue
3. filtrationThe precipitate was collected by filtration
4. washwashed with water
5. washThe obtained pale-brown solid was washed with a mixed solvent of ethyl acetate/hexane (1:1)