反应详情

A solution of 3,5-dinitroaniline (10 g, 54.644 mmol) and 2,5-dimethoxytetrahydrofuran (18.05 g, 136.61 mmol, 2.5 eq.) in acetic acid (122 ml) was heated to 100° C. for 16 h. Completion of reaction was monitored by TLC. Then the mixture was brought to RT and poured into ice-cold water. The precipitate was filtered, washed with water (150 ml) and dried to give the product in 54% yield (8.2 g). LC-MS (ESI): Calculated mass: 233.18; Observed mass: 233.04 [M+H]+ (rt: 1.667 min).

1. customCompletion of reaction
2. customwas brought to RT
3. additionpoured into ice-cold water
4. filtrationThe precipitate was filtered
5. washwashed with water (150 ml)
6. customdried
7. customto give the product in 54% yield (8.2 g)
8. custom233.04 [M+H]+ (rt: 1.667 min)