反应详情

To a suspension of 4.4 g (16.19 mmol) of 4-amino-2-azido-3-chloro-5-nitro-benzoic acid methyl ester in 161 mL of a mixture EtOH:MeOH 2:1 (v/v), 161 mL of a saturated NH4Cl aqueous solution is added followed by the addition of 88 mL of THF. Then 5.2 g (81 mmol) of powdered zinc is added and the reaction is stirred at ambient temperature during 5 h. The suspension is diluted with CH2Cl2 and the organic phase is washed with brine (2 times) and then dried on Na2SO4. After filtration and evaporation 3.2 g (14.84 mmol, 92%) of a dark violet-red solid were obtained and used directly in the next step without more purification. LC/MS: 216/218 (M+1)+

1. additionis added
2. washthe organic phase is washed with brine (2 times)
3. customdried on Na2SO4
4. filtrationAfter filtration
5. customwere obtained
6. customused directly in the next step without more purification