反应 #1563902
ord-612f92f895c345358aa006852407f27c
反应方程式
(6-Iodobenzo[d][1,3]dioxol-5-yl)methanol
PCC
→
6-iodobenzo[d][1,3]dioxole-5-carbaldehyde
收率 77.0%
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他After reaction
- 2其他the crude product was purified by column chromatography on silica gel (petroleum ether)
实验过程
(6-Iodobenzo[d][1,3]dioxol-5-yl)methanol (2.7 g, 9.7 mmol) in dry CH2Cl2 was added dropwise to PCC (3.1 g, 14.6 mmol) in dry CH2Cl2 at 0° C. under N2 atmosphere. The mixture was stirred at room temperature for 20 h. After reaction, the crude product was purified by column chromatography on silica gel (petroleum ether) to obtain 6-iodobenzo[d][1,3]dioxole-5-carbaldehyde (2 g, 77%) as white solid. LCMS: 277[M+1]+; 1H NMR (DMSO-d6) δ 6.20 (s, 2H), 7.28 (s, 1H), 7.61 (s, 1H), 9.79 (s, 1H).