反应 #2286303

反应方程式

2-[3,5-dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol

2-[3,5-Dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol

sodium acetate

acetic acid

→

acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester

收率 100.0%

Acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester

收率 100.0%

反应条件

后处理

1. 1
   温度At this time, the reaction mixture was cooled to room temperature
2. 2
   浓缩was concentrated under vacuum
3. 3
   workup.ADDITIONThe resulting residue was diluted with methylene chloride (25 mL)
4. 4
   洗涤was washed with water (10 mL)
5. 5
   其他The organic layer was separated
6. 6
   洗涤was washed with a saturated aqueous sodium bicarbonate solution (10 mL)
7. 7
   萃取extracted with methylene chloride (10 mL)
8. 8
   干燥dried with sodium sulfate
9. 9
   过滤filtered
10. 10
    浓缩concentrated
11. 11
    其他dried under high vacuum overnight

实验过程

A solution of 2-[3,5-dichloro-4-(6-chloro-5-isopropyl-pyridazin-3-yloxy)-phenyl]-ethanol (17) (500 mg, 1.38 mmol) in glacial acetic acid (5 mL) was treated with sodium acetate (230 mg, 2.8 mmol) and heated to 114° C. for 24 h. At this time, the reaction mixture was cooled to room temperature and was concentrated under vacuum. The resulting residue was diluted with methylene chloride (25 mL) and was washed with water (10 mL). The organic layer was separated and was washed with a saturated aqueous sodium bicarbonate solution (10 mL). The waters layers were combined and extracted with methylene chloride (10 mL). The organic layers were combined and dried with sodium sulfate, filtered, concentrated and dried under high vacuum overnight to afford acetic acid 2-[3,5-dichloro-4-(5-isopropyl-6-oxo-1,6-dihydro-pyridazin-3-yloxy)-phenyl]-ethyl ester (34) (531 mg, 100%) as a white solid; LRMS for C17H18Cl2N2O4 (M+) m/z=385 Molecular Weight=385.2500; Exact Mass=384.0644

来源