反应详情

温度

25 °C

The crude (1S,2R)-2-(4-fluoro-benzylamino)-cyclohexanecarboxylic acid methyl ester (4.97 mmol) was dissolved in N,N-dimethylformamide (40 mL) at 25° C. and (7-methanesulfonylamino-1,1-dioxo-1,4-dihydro-1λ6-benzo[1,2,4]thiadiazin-3-yl)-acetic acid (prepared as described in Example 1j, 1.47 g, 4.41 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (0.887, 4.63 mmol), and N-methylmorpholine (1.01 mL, 9.19 mmol) were added sequentially. The reaction mixture was stirred at 25° C. for 2 h, and then was concentrated in vacuo. The residue was partitioned between 1.0 M aqueous hydrochloric acid solution (150 mL) and ethyl acetate (2×150 mL). The combined organic layers were dried over sodium sulfate, decanted, and were concentrated in vacuo to afford the crude product, (1S,2R)-2-{(4-fluoro-benzyl)-[2-(7-methanesulfonylamino-1,1-dioxo-1,4-dihydro-1λ6-benzo[1,2,4]thiadiazin-3-yl)-acetyl]-amino}-cyclohexanecarboxylic acid methyl ester as a yellow oil, which was used directly in the next step without further purification.

1. concentrationwas concentrated in vacuo
2. customThe residue was partitioned between 1.0 M aqueous hydrochloric acid solution (150 mL) and ethyl acetate (2×150 mL)
3. dry with materialThe combined organic layers were dried over sodium sulfate
4. customdecanted
5. concentrationwere concentrated in vacuo