反应详情

温度

40 °C

The product of step c) (74.2 mg, 0.30 mmol) was placed in a vial and diluted with CHCl3 (740 μl) and AcOH (740 μl). Next, hydroquinone (−5 mg) was added followed by NCS (41.3 mg, 0.31 mmol) and the contents were heated to 40° C. for 6 hours. The crude reaction mixture was diluted with water (2 ml) and extracted with EtOAc (3×3 ml). The organic layer was dried (MgSO4) and purified by preparative TLC using hexanes/EtOAc 50:50 providing subtitled product. MS calculated for C13H16ClNO2S+H 286, observed 286.

1. customThe crude reaction mixture
2. extractionextracted with EtOAc (3×3 ml)
3. dry with materialThe organic layer was dried (MgSO4)
4. custompurified by preparative TLC