HRID970038
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a suspension of 1-acetyl-5-aminoindoline (130 mg, 0.74 mmol) in anhydrous THF (10 mL) was added LiAlH4 (42 mg, 1.11 mmol). The mixture was stirred at rt for 6 h, quenched with saturated NH4Cl and extracted with ethyl acetate. The organic phase was washed with brine, dried over sodium sulphate and concentrated in vacuo to give a purple residue (80 mg, 67%) that was used without further purification. 1H NMR (270 MHz, DMSO): δ 6.56 (1H, s, ArH), 6.47 (1H, d broad, J=8.1 Hz, ArH), 6.37 (1H, d, J=8.0 Hz, ArH), 3.29 (2H, s, NH2), 3.20 (2H, t, J=7.6 Hz, CH2), 3.02 (2H, q, J=6.9 Hz, CH2), 2.86 (2H, t, J=7.6 Hz, CH2), 1.17 (3H, t, J=6.9 Hz, CH3).
WORKUP
后处理
- customquenched with saturated NH4Cl
- extractionextracted with ethyl acetate
- washThe organic phase was washed with brine
- dry with materialdried over sodium sulphate
- concentrationconcentrated in vacuo