反应详情

10.00 g of 3-bromobenzylamine hydrochloride suspended in chloroform (100 ml) was mixed with 9.55 g of triethylamine at room temperature. The resulting solution was stirred under cooling with ice while 4.67 g of methyl chloroformate was added dropwise and then stirred at room temperature for 2 hours. After the reaction, the reaction solution was poured into saturated aqueous sodium chloride, and the organic layer was separated, dried over anhydrous magnesium sulfate and evaporated at ordinary pressure for removal of the solvent. The residue was purified by silica gel column chromatography to give 9.54 g of methyl N-(3-bromobenzyl)carbamate as white crystals. m.p. 41-44° C.

1. additionwas added dropwise
2. stirringstirred at room temperature for 2 hours
3. customAfter the reaction
4. customthe organic layer was separated
5. dry with materialdried over anhydrous magnesium sulfate
6. customevaporated at ordinary pressure for removal of the solvent
7. customThe residue was purified by silica gel column chromatography