反应详情

550 mg (2.00 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-benzo[d][1,3]diazepin-2-one, 610 mg (1.80 mmol) 6-(3.6-dichloro-pyridazine-4-carbonyl)-3,4-dimethyl-3H-benzoxazol-2-one, 630 mg (4.39 mmol) copper(I)bromide and 430 mL (2.50 mmol) DIPEA in 5 mL DMF were stirred for 2 h at 110° C., then cooled and filtered. The filtrate was combined with 1 mL of a 1N aqueous hydrochloric acid solution and precipitated with 40 mL ice water. The precipitate was suction filtered, washed with water and dried. The solid was stirred with 120 mL DCM/MeOH (11:1), filtered through silica gel and washed with DCM/MeOH. The filtrate was evaporated down. The residue was triturated with diethyl ether, suction filtered and dried. A mixture of isomers was obtained which was further reacted.

1. temperaturecooled
2. filtrationfiltered
3. customprecipitated with 40 mL ice water
4. filtrationfiltered
5. washwashed with water
6. customdried
7. filtrationfiltered through silica gel
8. washwashed with DCM/MeOH
9. customThe filtrate was evaporated down
10. customThe residue was triturated with diethyl ether, suction
11. filtrationfiltered
12. customdried
13. additionA mixture of isomers
14. customwas obtained which