反应详情

温度

80 °C

A mixture of 1-bromo-2-chloro-5-iodo-4-methoxybenzene (3 g, 8.64 mmol), (S)-2-aminopropanoic acid (769 mg, 8.64 mmol), CuI (164 mg, 0.864 mmol), 2-hydroxybenzaldehyde phenylhydrazone (366 mg, 1.73 mmol), K3PO4.3H2O (4.6 g, 17.28 mmol) in DMF (10 mL) was stirred under argon at 80° C. for 16 h. The mixture was allowed to cool to RT, H2O and Et2O were added to the solution. The resulting solution was partitioned into two phases, the aqueous phase was separated, and the organic layer was extracted with 5% NaOH. The combined aqueous phase was acidified to pH 4 with 20% HCl, and then extracted with Et2O. The resulting organic layer was dried over MgSO4 and concentrated in vacuo to afford the desired product (1.7 g, 64% yield). ESI-MS m/z: 306.1[M+H]−

1. temperatureto cool to RT
2. customThe resulting solution was partitioned into two phases
3. customthe aqueous phase was separated
4. extractionthe organic layer was extracted with 5% NaOH
5. extractionextracted with Et2O
6. dry with materialThe resulting organic layer was dried over MgSO4
7. concentrationconcentrated in vacuo