反应详情

温度

0 °C

4.41 g (8.72 mmol) {(S)-6-[(R)-7-fluoro-4-(4,4,5,5-tetramethyl-[1,3,2]dioxaborolan-2-yl)-indan-1-yloxy]-2,3-dihydrobenzofuran-3-yl}-acetic acid methyl ester is dissolved in 10 ml EtOH and 2.20 ml glacial acetic acid and 2.20 ml water are added. The funnel is rinsed with 7.50 ml EtOH. Then, 2.28 g (14.8 mmol) sodium perborate is added in portions at r.t. and the mixture is stirred. After complete addition, 1.40 ml water and 1.6 ml toluene is added. The organic phase is separated and 1.60 ml water is added. After cooling to 0° C., the 2-phasic mixture is seeded and stirring is continued. The precipitated product is filtered off, washed with cold toluene and dried. Yield: 2.86 g; Rf=0.22 (silica gel, PE/EtOAc=7/3); Mass spectrum (ESI): m/z=359 [M+H]+.

1. washThe funnel is rinsed with 7.50 ml EtOH
2. additionis added
3. customThe organic phase is separated
4. addition1.60 ml water is added
5. stirringstirring
6. filtrationThe precipitated product is filtered off
7. washwashed with cold toluene
8. customdried