反应详情

To a solution of 20 (0.19 g, 0.32 mmol) in methanol:dimethylformamide 1:1 (4 mL), acetic acid was added (0.114 mL, 1.9 mmol) followed by potassium fluoride (0.110 mg, 1.9 mmol). The mixture was stirred for 30 hours then diluted with tertbutylmethyl ether (50 mL) and washed with water (20 mL) then brine (20 mL), then dried over sodium sulphate. The solvent was removed under reduced pressure to give a crude which was purified by column (cyclohexane:AcOEt 7:3+1% AcOH) to give 0.097 g of ZSB-74:

1. washwashed with water (20 mL)
2. dry with materialbrine (20 mL), then dried over sodium sulphate
3. customThe solvent was removed under reduced pressure
4. customto give a crude which
5. customwas purified by column (cyclohexane:AcOEt 7:3+1% AcOH)
6. customto give 0.097 g of ZSB-74