Imidazole → HCID 13600632, compound

A mixture of Ph3P (3.205 g, 12.2 mmol), imidazole (1.221 g, 17.9 mmol), and I2 (3.024 g, 11.9 mmol) in CH2Cl2 (38 mL) was stirred at room temperature. After 15 min., a solution of 7-2 (1.283 g, 10.0 mmol) in CH2Cl2 (4.8 mL) was added by cannula, rinsing with 4 mL CH2Cl2. After 3 h, the mixture was filtered through basic alumina, washing with 10% ethyl acetate/hexanes. The filtrate was evaporated and the residue was purified by flash chromatography on silica gel (Isco Combiflash unit) to provide the title compound (2.323 g, 98%).

1. washrinsing with 4 mL CH2Cl2
2. waitAfter 3 h
3. filtrationthe mixture was filtered through basic alumina
4. washwashing with 10% ethyl acetate/hexanes
5. customThe filtrate was evaporated
6. customthe residue was purified by flash chromatography on silica gel (Isco Combiflash unit)

ORD record

ord-97c03bc4e94e406fa9198b22a637883f

Source dataset

uspto-grants-2015_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09006464B2