反应详情

To a cold (−70° C.) solution of oxalyl chloride (0.27 mL, 3.06 mmol) in dichloromethane (15 mL) is added DMSO (0.32 mL, 6.11 mmol) followed by the alcohol 256 (1.28 g, 2.48 mmol) in dichloromethane (5 mL). The mixture is stirred for at −70° C. solution 15 min., and triethylamine (1.03 mL, 13.9 mmol) is added and the mixture is allowed to come to RT and is stirred for 4 h. The reaction mixture is washed with water, brine, then dried (MgSO4), and filtered. The filtrate is rotary evaporated, and the residue is recrystallized from Et2O to give 1.02 g of the product 257. 1H NMR (CDCl3) δ 10.60 (s, 1H), 8.10-7.95 (m, 2H), 7.10-6.90 (m, 12H), 6.90-6.70 (m, 2H), 5.40 (s, 2H), 1.25 (s, 9H); MS: m/z 459 (M++1).

1. additionis added
2. customto come to RT
3. washThe reaction mixture is washed with water, brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customthe residue is recrystallized from Et2O