tert-Butanol → HCID 18382719、化合物

反応式

[C:1]([C:3]1[C:8]([CH3:9])=[CH:7][C:6]([CH3:10])=[CH:5][N:4]=1)#[N:2].[C:11](O)([CH3:14])([CH3:13])[CH3:12].[OH-:16].[Na+]>S(=O)(=O)(O)O>[CH3:12][C:11]([NH:2][C:1]([C:3]1[C:8]([CH3:9])=[CH:7][C:6]([CH3:10])=[CH:5][N:4]=1)=[O:16])([CH3:14])[CH3:13]

参加物

反応条件

温度: 75 °C

実験手順

To a stirred solution of 20.3 g (0.153 mol) of 2-cyano-3,5-dimethylpyridine in 100 mL of 20 mL of conc. sulfuric acid within 10 minutes, followed by 20 mL of t-butanol over an additional 15 minutes. The solution was warmed at 75° C. for 30 minutes after which it was cooled to room temperature and basified with 25% NaOH. The product was extracted 3× with EtOAc (600 mL), which was combined and washed 1× with brine, dried (Na2SO4), filtered and concentrated in vacuo to give the title compound (31.26 9) as a yellowish oil.