反应详情

NaH (24 mg, 0.50 mmol) was added slowly to a solution of 84AF84-19 (0.149 g, 0.41 mmol) in dry DMF (5 mL) and the mixture stirred at rt for 30 min. A solution of 4-isobutoxybenzyl bromide 69NLS69 (117 mg, 0.48 mmol) in dry DMF (1 mL) was added dropwise to the mixture. After 1 h stirring at rt the mixture was partitioned between ethyl acetate and water. The organic layer was dried over sodium sulphate, filtered and concentrated in vacuo. Purification of the residue by column chromatography on silica gel, eluting with a stepwise gradient of 3-6% methanol in dichloromethane, followed by preparative reversed phase HPLC (C18) afforded the desired compound (109 mg, 50%).

1. stirringAfter 1 h stirring at rt the mixture
2. customwas partitioned between ethyl acetate and water
3. dry with materialThe organic layer was dried over sodium sulphate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification of the residue by column chromatography on silica gel
7. washeluting with a stepwise gradient of 3-6% methanol in dichloromethane