反应详情

A solution of 3-aminobenzoic acid (0.5 g; 3.8 mmol) and N-ethyldiisopropylamine (DIEA) (0.64 mL; 3.8 mmol) in THF (20 mL) was added dropwise to a solution of Fmoc-glycine chloride (1.2 g; 4.0 mmol) (3) in THF (10 mL) and CH2Cl2 (10 mL). After 24 h stirring at room temperature 1 M HCl (50 mL) was added (final pH: 1.5). The precipitate was filtered, washed with H2O (2×100 mL), vacuum dried and crystallised from CHCl3/CH3OH (1:1) to give B as a white solid (0.7 g; 1.6 mmol). Yield 43%.

1. additionwas added (final pH: 1.5)
2. filtrationThe precipitate was filtered
3. washwashed with H2O (2×100 mL), vacuum
4. customdried
5. customcrystallised from CHCl3/CH3OH (1:1)
6. customto give B as a white solid (0.7 g; 1.6 mmol)