反应详情

0.84 g (5.00 mmol) 4-amino-3-methyl-5-nitro-phenol, 0.58 g (5.00 mmol) (R)-tetrahydro-furan-2-carboxylic acid, 1.77 g (5.50 mmol) TBTU and 1.92 mL (11.00 mmol) DIPEA in 10.0 mL DMF were stirred overnight at RT. The reaction mixture was poured onto ice water and extracted with ethyl acetate. The organic phase was separated off, dried and evaporated down i.vac. The residue was purified by preparative HPLC-MS. The fractions containing product were partially evaporated down i.vac. and neutralised with an aqueous 1M sodium hydroxide solution. The precipitate formed was suction filtered, washed and dried.

1. additionThe reaction mixture was poured onto ice water
2. extractionextracted with ethyl acetate
3. customThe organic phase was separated off
4. customdried
5. customevaporated down i.vac
6. customThe residue was purified by preparative HPLC-MS
7. additionThe fractions containing product
8. customwere partially evaporated down i.vac
9. customThe precipitate formed
10. filtrationfiltered
11. washwashed
12. customdried