反应详情

温度

100 °C

To a mixture of 8-chloro-10H-dibenzo[b,f][1,4]thiazepin-11-one (189JO13) (38 mg, 0.15 mmol) and N,N-dimethylaniline (46 μL, 0.36 mmol) in toluene was added POCl3 (27 μL, 0.29 mmol) and the resulting mixture was stirred for 2 h at 100° C., and then concentrated. Toluene (2 mL) and piperazine (62 mg, 0.73 mmol) were added, and the resulting mixture was stirred at 100° C. for 3 h, and then allowed to obtain room temperature. To the mixture was added aqueous HCl (1 mL, 2 M) and then the aqueous phase was extracted with EtOAc (2×2 mL). To the aqueous phase was added aqueous NaOH (3 mL, 2 M) and the resulting mixture was extracted with EtOAc (3×3 mL). The combined organic phases were concentrated and purified by HPLC to give 6.6 mg of the title compound (189JO16). MS (ESI) 330 (MH+). Purity for MH+ (UV/MS) 99/98.

1. concentrationconcentrated
2. stirringthe resulting mixture was stirred at 100° C. for 3 h
3. customto obtain room temperature
4. extractionthe aqueous phase was extracted with EtOAc (2×2 mL)
5. additionTo the aqueous phase was added aqueous NaOH (3 mL, 2 M)
6. extractionthe resulting mixture was extracted with EtOAc (3×3 mL)
7. concentrationThe combined organic phases were concentrated
8. custompurified by HPLC