反应详情

温度

80 °C

A mixture of 5-chloro-1-indanone (1.05 g, 6.28 mmol) and N-bromosuccinimide (2.23 g, 12.56 mmol) in DMSO (25 ml) was stirred overnight at 40° C. and 5 h at 80° C. under vacuum. Water (125 ml) was added and the mixture was extracted with CH2Cl2 (25 ml). The aqueous phase was saturated with brine and solid NaCl and extracted with CH2Cl2 (4×80 ml). The collected organic phases were dried over Na2SO4 and the solvent evaporated. The crude was dissolved in EtOH (63 ml), diaminomaleonitrile (678 mg, 6.28 mmol) and a catalytic amount of AcOH were added and the mixture stirred at 80° C. for 45 min. The precipitate was collected by filtration and washed with EtOH (464 mg). The filtered solution was evaporated and the crude purified by flash.

1. extractionthe mixture was extracted with CH2Cl2 (25 ml)
2. extractionextracted with CH2Cl2 (4×80 ml)
3. dry with materialThe collected organic phases were dried over Na2SO4
4. customthe solvent evaporated
5. dissolutionThe crude was dissolved in EtOH (63 ml)
6. stirringthe mixture stirred at 80° C. for 45 min
7. filtrationThe precipitate was collected by filtration
8. washwashed with EtOH (464 mg)
9. customThe filtered solution was evaporated
10. customthe crude purified by flash