2-Chlorophenothiazine → 1-propan-2-yl-10H-phenothiazine
反応式
Cl[C:2]1[CH:15]=[CH:14][C:13]2[S:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[NH:5][C:4]=2[CH:3]=1.[CH2:16]1[CH2:20]OC[CH2:17]1>>[CH:16]([C:3]1[C:4]2[NH:5][C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[S:12][C:13]=2[CH:14]=[CH:15][CH:2]=1)([CH3:20])[CH3:17]参加物
3
実験手順
To a solution of 2-chlorophenothiazine (4.67 g, 20 mmol) in anhydrous THF (40 mL) i-propyllithium (0.7 m solution in pentane, 100 mL, 70 mmol) was added at −75° C. (1 h). The reaction mixture had been stirred (2 h), ice-water was added slowly (30 min.) and after that the stirring was continued for 30 min. The organic layer was separated and combined with ether extracts of the aqueous phase. The combined organic phase was washed with water, dried (Na2SO4) and concentrated to give the crude product (52% yield). Compound was purified by flash chromatography (solvent system: hexane-ethyl acetate).
後処理
- additionwas added slowly (30 min.)
- customThe organic layer was separated
- washThe combined organic phase was washed with water