反应详情

A solution of 3-[(1-tert-butoxycarbonyl-cyclobutylmethyl)-sulfamoyl]-benzoic acid methyl ester (step 3) (1.87 g, 4.88 mmol) in THF (25 ml) was treated with 2M NaOH (aq) (24.38 ml, 48.8 mmol) and stirred at RT for 2 h. The reaction mixture was partitioned between diethyl ether and water. The aqueous portion was separated and acidified to pH 1 with 2N HCl, and extracted with EtOAc, and the combined organic portions were washed with brine, dried over MgSO4 and concentrated in vacuo to afford the title product; 1H NMR (400 MHz, CDCl3) δ 8.64 (1H, s), 8.33 (1H, d), 8.12 (1H, d), 7.67 (1H, t), 5.40 (1H, t), 3.24 (2H, d), 2.38 (2H, m), 1.97 (4H, m), 1.48 (9H, s). LC-MS Rt 1.13 mins; 314.1 [M+H]+ (−tBu), Method 2minLC_v003.

1. customThe reaction mixture was partitioned between diethyl ether and water
2. customThe aqueous portion was separated
3. extractionextracted with EtOAc
4. washthe combined organic portions were washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo