反应详情

温度

0 °C

To a round bottom flask equipped with a magnetic stirrer and addition funnel were added tosyl bromide (30.6 g, 130 mmol), CCl4 (150 mL), and pyridine (10.51 mL, 130 mmol), respectively. This slurry was cooled to 0° C. and treated dropwise a solution of 24.3 g (124 mmol) of 5-tert-butyl-4-mercapto-2-methyl-phenol (prepared in Example QQQ) in CCl4 (150 mL). The mixture was diluted with CHCl3, washed with brine, and dried (MgSO4). The solvent was evaporated to give a solid which was washed and filtered with hexanes:Et2O (4:1) to give the title compound. 1H NMR (CDCl3) δ 1.22 (s, 9 H), 2.11 (s, 3 H), 2.42 (s, 3 H), 6.87 (s, 1 H), 7.16 (s, 1 H) 7.26 (d, 2 H), 7.49 (d, 2 H).

1. customTo a round bottom flask equipped with a magnetic stirrer and addition funnel
2. washwashed with brine
3. dry with materialdried (MgSO4)
4. customThe solvent was evaporated
5. customto give a solid which
6. washwas washed
7. filtrationfiltered with hexanes:Et2O (4:1)