反应详情

温度

3 °C

Nicotinoyl chloride hydrochloride (7.12 g) is added to a solution of 3-(2-aminothiazol-5-yl)-2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene (11.3 g) in tetrahydrofuran (300 cc), cooled to 3° C., and triethylamine (11.12 cc) is then added in the course of 10 minutes. The mixture is stirred for 1 hour at 3° C. and then for 2 hours while allowing the temperature to ri$e to 20° C. The reaction mixture is poured into ethyl acetate (400 cc) and washed with distilled water (3×120 cc) and a saturated solution of sodium chloride (100 cc). The organic phase is dried and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. The residue is crystallised from ethyl acetate (20 cc) to give 2-benzhydryloxycarbonyl-7-t-butoxycarbonylamino-3-(2-nicotinoylaminothiazol-5-yl)-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene (7.4 g) in the form of a yellow solid.

1. waitfor 2 hours while allowing
2. customto ri$e to 20° C
3. washwashed with distilled water (3×120 cc)
4. customThe organic phase is dried
5. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C
6. customThe residue is crystallised from ethyl acetate (20 cc)