反应详情

3,5-Trans-N-(2-fluorobenzyl)-5-(2-tert-butoxycarbonylaminomethylphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetamide (1) A tetrahydrofuran (30 ml) solution of N-methyl-N-methyloxy-2-amino-5-chlorobenzamide (4.3 g) and N-tert-butoxycarbonyl-2-bromobenzylamine (3.82 g) was cooled to −78° C. To the solution was gradually added dropwise a hexane solution of n-butyl lithium (1.6 mol/L) (42 ml). To the mixture were then added water (100 ml) and acetic acid ethyl ester (100 ml). The organic layer was washed with water and dried over anhydrous MgSO4. The solvent was then distilled off. The residual oily compound was purified by means of a silica gel column chromatography to give a yellow solid product, which was recrystallized from n-hexane-isopropyl ether. The crystals were collected by filtration to afford 2-amino-2′-tert-butoxycarbonylaminomethyl-5-chlorobenzophenone (1.3 g) as a pale yellow crystalline product.

1. washThe organic layer was washed with water
2. dry with materialdried over anhydrous MgSO4
3. distillationThe solvent was then distilled off
4. customThe residual oily compound was purified by means of a silica gel column chromatography
5. customto give a yellow solid product, which
6. customwas recrystallized from n-hexane-isopropyl ether
7. filtrationThe crystals were collected by filtration