反应详情

Combine 2-bromo-5-trifluoromethylphenylamine (27.06 g, 112.74 mmol) and 200 mL of pyridine. Cool in an ice bath and add ethyl chloroformate (18.35 g, 169.11 mL, 1.5 eq). After addition was complete, allow the reaction to gradually warming to room temperature. After 18 hours, evaporate it vacuo to give a residue. Dissolve the residue in Et2O/water and transfer to a separatory funnel. Separate the layer and extract the aqueous layer with Et2O (2×300 mL), combine the organic layers, dry over MgSO4, filter, and evaporate in vacuo to give N-(2-bromo-5-trifluoromethylphenyl)carbamic acid ethyl ester which may be used without further purification.

1. temperatureCool in an ice bath
2. additionAfter addition
3. customthe reaction
4. customevaporate it vacuo
5. customto give a residue
6. customSeparate the layer
7. extractionextract the aqueous layer with Et2O (2×300 mL)
8. dry with materialdry over MgSO4
9. filtrationfilter
10. customevaporate in vacuo