反应详情

CAS #1252633-25-2 (5.3 g, 12.3 mmol, Eq: 1.00) was dissolved in propionitrile (40 ml) and 4-bromo-2-chlorobenzenethiol (3.3 g, 14.8 mmol, Eq: 1.20) was added. Now triethyl amine (2.49 g, 3.43 ml, 24.6 mmol, Eq: 2.00) was added. The reaction mixture was stirred at reflux over night. The reaction mixture was poured into 100 ml 10% Na2CO3 and extracted with EtOAc (2×100 mL). The organic layer was extracted with 100 ml 0.1N HCl, dried over Na2SO4, filtered and evaporated. The crude material was purified by flash chromatography (silica gel, 120 g, 0% to 30% AcOEt in heptane in 30 min) to yield a colorless oil (4.72 g; 85%). m/z=352.1 [M+H-Boc]+.

1. temperatureat reflux over night
2. extractionextracted with EtOAc (2×100 mL)
3. extractionThe organic layer was extracted with 100 ml 0.1N HCl
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. customevaporated
7. customThe crude material was purified by flash chromatography (silica gel, 120 g, 0% to 30% AcOEt in heptane in 30 min)
8. customto yield a colorless oil (4.72 g; 85%)