反应详情

A solution of 4-Chloro-7-(4-methoxy-benzyl)-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidine (0.36 g, 1.31 mmol), 1-Boc-piperazine (1.0 g, 5.37 mmol) and tBuOK (0.18 g, 1.60 mmol) in NMP (20 mL) was heated to 128° C. for 20 hours. After cooling, the mixture was diluted with ethyl acetate (500 mL) and washed with water (5×150 mL). The organic phase was dried and concentrated. The residue was subject to column chromatography, eluted by hexane/ethyl acetate (1:1) to give 4-[7-(4-Methoxy-benzyl)-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl]-piperazine-1-carboxylic acid tert-butyl ester (0.32 g, 57%). 1H NMR (CDCl3, 400 MHz) δ 8.17 (s, 1H), 7.20 (d, J=8.4 Hz, 2H), 6.84 (d, J=8.4 Hz, 2H), 4.50 (s, 2H), 3.79 (s, 3H), 3.59 (m, 4H), 3.48 (m, 4H), 3.35 (m, 2H), 3.30 (m, 2H), 1.49 (s, 9H). MS (APCI+) [M+H]+426.

1. temperatureAfter cooling
2. washwashed with water (5×150 mL)
3. customThe organic phase was dried
4. concentrationconcentrated
5. washeluted by hexane/ethyl acetate (1:1)