反应 #171759

反应方程式

2,4-difluorophenylhydrazine hydrochloride

9-bromo-4,5-dihydro-6-oxa-1-thia-benzo[e]azulene-2-carboxylic acid amide

dimethylformamide dimethyl acetal

toluene

→

293

3-(9-bromo-4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)-4-(2,4-difluorophenyl)-4H-1,2,4-triazole

溶剂

water

dichloromethane

acetic acid

反应条件

后处理

1. 1
   温度The reaction mixture was heated to 100° C. for 3 hours
2. 2
   温度The reaction mixture was then cooled
3. 3
   洗涤washed with sodium carbonate solution
4. 4
   干燥dried (MgSO4)
5. 5
   其他the solvent removed in vacuo
6. 6
   其他Purification

实验过程

A mixture of 9-bromo-4,5-dihydro-6-oxa-1-thia-benzo[e]azulene-2-carboxylic acid amide (340 mg), dimethylformamide dimethyl acetal (3 ml) and toluene (2.5 mL) was heated to 100° C. for 16 hours. The solvent was then reduced in vacuo and dissolved in acetic acid (3 ml) and water (0.3 mL) and to this was added 2,4-difluorophenylhydrazine hydrochloride (265 mg). The reaction mixture was heated to 100° C. for 3 hours. The reaction mixture was then cooled, and then diluted with dichloromethane, washed with sodium carbonate solution, dried (MgSO4) and the solvent removed in vacuo. Purification using flash chromatography yielded 293. NMR: (CDCl3): 3.15 (2H, t), 4.31 (2H, t), 6.82 (1H, d), 6.86 (1H, s), 7.08-7.13 (2H, m), one proton under chloroform peak, 7.72 (1H, s), 8.10 (1H, s)

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