反应详情

温度

90 °C

(4-Mercaptophenyl)methanol (2.38 g, 17.0 mmol) and 53B (5.00 g, 15.5 mmol) were mixed in DMF (80 mL). Cs2CO3 (6.05 g, 18.56 mmol) was added. The mixture was stirred at 90° C. overnight and then cooled room temperature. Ethyl acetate (150 mL) was added and the mixture was washed with water (50 mL). The aqueous layer was extracted with ethyl acetate (100 mL). The organic phases were combined, dried (MgSO4) and evaporated to dryness. The residue was purified by column chromatography eluting with ethyl acetate/heptane (20:80, 40:60 and then 60:40). There was obtained 3.5 g (61%) of 60A as a solid. 1H NMR (500 MHz, CDCl3): δ 4.19 (m, 2H), 4.64 (m, 2H), 4.69 (s, 2H), 5.10 (m, 1H), 7.34 (m, 4H), 7.53 (t, 2H), 7.59 (t, 1H), 8.15 (d, 2H), MS (APCI+) m/z 368 [M−H]+.

1. temperaturecooled room temperature
2. washthe mixture was washed with water (50 mL)
3. extractionThe aqueous layer was extracted with ethyl acetate (100 mL)
4. dry with materialdried (MgSO4)
5. customevaporated to dryness
6. customThe residue was purified by column chromatography
7. washeluting with ethyl acetate/heptane (20:80, 40:60