反应详情

温度

-78 °C

To a solution of (S)-2-(7-bromo-2-hydroxy-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyethyl pivalate (67B) (40 mg, 0.090 mmol) in THF (1 ml) was added KOtBu (0.14 ml, 0.135 mmol, 1M in THF) slowly at −78° C. After 15 min, MeI (8.5 ul, 0.135 mmol) was added at −78° C. and stirred at −78° C. for 15 min. Then the reaction was reacted at rt for 3 hs. The reaction mixture was washed by sat. NaHCO3, extracted by EtOAc, dried over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-40% EtOAc in hexanes to give 67C (30 mg, 73%).

1. customThen the reaction was reacted at rt for 3 hs
2. washThe reaction mixture was washed by sat. NaHCO3
3. extractionextracted by EtOAc
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated down
7. custompurified by silica gel column
8. washeluting by 0-40% EtOAc in hexanes