反应详情

温度

100 °C

2.00 mL (27.4 mmol) thionyl chloride were added to 1.92 g (9.95 mmol) 3,6-dichloro-pyridazine-4-carboxylic acid in 10 mL 1,2-dichloroethane and the mixture was refluxed for 2 h. The reaction mixture was evaporated to dryness and coevaporated with 1,2-dichloroethane. Then 5.30 g (39.8 mmol) aluminium trichloride and 1.56 g (10.5 mmol) 4-methyl-3H-benzoxazol-2-one were added and the mixture was stirred for 1 h at 100° C. under a nitrogen atmosphere. Then it was stirred for a further 2 h at 120° C., 3 h at 130° C. and then cooled for 48 h at RT. The mixture was decomposed with ice water and extracted with DCM. The organic phases were combined, washed with water, dried on sodium sulphate, filtered and evaporated down i. vac. The residue was triturated with DIPE, suction filtered and dried.

1. temperaturethe mixture was refluxed for 2 h
2. customThe reaction mixture was evaporated to dryness
3. stirringThen it was stirred for a further 2 h at 120° C., 3 h at 130° C.
4. temperaturecooled for 48 h at RT
5. extractionextracted with DCM
6. washwashed with water
7. customdried on sodium sulphate
8. filtrationfiltered
9. customevaporated down i
10. customThe residue was triturated with DIPE, suction
11. filtrationfiltered
12. customdried