反应详情

4.6 ml (33 mmoles) of triethylamine is added to a solution of 1.82 g (10 mmoles) of L-Leucine methyl ester hydrochloride, 2.43 g (10 mmoles) of 10H-phenothiazine-2-carboxylic acid (J. Med. Chem.(1998) 41 (2), 148-156), 1.48 g (11 mmoles) of HOBT and 4.21 g (22 mmoles) of EDC in 30 ml of anhydrous DMF. The reaction mixture is stirred for 15 hours. After evaporation of the solvent under vacuum, the residue is divided between 100 ml of AcOEt and 50 ml of a 1M solution of HCl. The organic phase is decanted and washed successively with 50 ml of H2O, 50 ml of a saturated solution of NaHCO3 and 50 ml of salt water. The organic solution is dried over magnesium sulphate, filtered and concentrated to dryness under vacuum. The evaporation residue is taken up in Et2O and filtered. Yellow powder (71%). Melting point: 160.5-161° C.

1. customAfter evaporation of the solvent under vacuum
2. customThe organic phase is decanted
3. washwashed successively with 50 ml of H2O, 50 ml of a saturated solution of NaHCO3 and 50 ml of salt water
4. dry with materialThe organic solution is dried over magnesium sulphate
5. filtrationfiltered
6. concentrationconcentrated to dryness under vacuum
7. filtrationfiltered