反应详情

To a stirred -78° C. solution of Ts-Leu (15 g, 53 mmol) in dry THF (240 ml) was added n-butyl lithium (57.8 ml of a 0.91M solution in hexane) followed 15 minutes later by isopentyl magnesium bromide (185 ml of a 0.8M solution in THF). The mixture was heated at reflux for 3 days, then cooled and poured into 0° C. 1M HCl (500 ml). The layers were separated and the aqueous phase was extracted with ether (3×150 ml). The combined organic layers were washed with saturated NaHCO3 (2×150 ml) and brine (150 ml). Drying and evaporating provided a residue which was chromatographed on silica gel to give 7.43 g (41%) of the desired product. Mass spectrum: (M+H)+ =340.

1. temperatureThe mixture was heated
2. temperatureat reflux for 3 days
3. temperaturecooled
4. additionpoured into 0° C
5. customThe layers were separated
6. extractionthe aqueous phase was extracted with ether (3×150 ml)
7. washThe combined organic layers were washed with saturated NaHCO3 (2×150 ml) and brine (150 ml)
8. customDrying
9. customevaporating
10. customprovided a residue which
11. customwas chromatographed on silica gel