反应详情

Methyl 2-(6-bromo-5-fluoro-1H-indol-1-yl)acetate (D77) (10.2 g, 35.7 mmol) was dissolved up in 81 mL of THF and cooled in a cardice/acetone bath before the addition of LiAlH4 (2N in THF solution) (17.83 mL, 35.7 mmol). The reaction mixture was left to stir in the cardice/acetone bath for 30 mins. Whilst still in the bath the reaction mixture was quenched by the dropwise addition of saturated sodium sulfate aqueous solution. The solid formed was filtered off and washed with ethyl acetate. The filtrate was washed with brine. The organic layer was passed through a hydrophobic frit and concentrated to afford title compound (8.852 g). LCMS (A): m/z (M+H)+ 258/260, C10H9BrFNO requires 257/259 (acidic).

1. waitThe reaction mixture was left
2. customWhilst still in the bath the reaction mixture was quenched by the dropwise addition of saturated sodium sulfate aqueous solution
3. customThe solid formed
4. filtrationwas filtered off
5. washwashed with ethyl acetate
6. washThe filtrate was washed with brine
7. concentrationconcentrated