反应详情

温度

100 °C

Add to 4H-thieno[3,2-b]pyrrole-5-carboxylic acid ethyl ester (1.74 gm, 8.9 mmol) and 7M ammonia in methanol (100 ml) in a steel bomb a chip of lithium hydroxide (0.1 gm). Seal the bomb and heat to 100° C. for 16 hrs. Cool to room temperature, and concentrate to remove the volatiles. Purify the crude product via flash chromatography (ISCO, silica cartridge, 40 gm, elute with methanol 0-5% in methylene chloride) to provide the title compound (560 mg, 38%) as an off-white solid.

1. customSeal the bomb
2. temperatureCool to room temperature
3. concentrationconcentrate
4. customto remove the volatiles
5. customPurify the crude product
6. washvia flash chromatography (ISCO, silica cartridge, 40 gm, elute with methanol 0-5% in methylene chloride)