反应详情

A procedure similar to that in Example 4 was used. 5-cyclohexylmethyl-4-(4-methoxy-phenyl)-thiazol-2-ylamine prepared in Example 47 and 3,4-dimethoxy-benzoyl chloride prepared in the step 1 of Example 12 were used as starting materials, allowed to react at room temperature overnight, followed by post-treatment to give a crude product, which was purified by a silica gel column chromatography eluted with a gradient of dichloromethane and ethyl acetate (20:1) to obtain a product as a white solid in a yield of 67.5%, mp: 171-172 └. 1H-NMR (CDCl3, 400 MHz) δ: 0.82˜0.98 (2H, m), 1.08˜1.28 (3H, m), 1.58˜1.88 (6H, m), 2.74 (2H, d, J=7.28 Hz, CHCH2Ar), 3.82 (3H, s, OCH3), 3.89 (3H, s, OCH3), 3.94 (3H, s, OCH3), 6.82˜6.89 (3H, m, ArH), 7.35˜7.47 (4H, m, ArH), 11.00 (1H, br, CONH); EI-MS m/e (%): 466.2 (M+, 46), 383.2 (29), 165.1 (100); HREI-MS Calcd. for C26H30N2O4S: 466.1926. found: 466.1920. Anal. Calcd. for C26H30N2O4S: C, 66.93; H, 6.48; N, 6.00. found: C, 66.88; H, 6.68; N, 6.02.

1. customto react at room temperature overnight
2. customto give a crude product, which
3. customwas purified by a silica gel column chromatography
4. washeluted with a gradient of dichloromethane and ethyl acetate (20:1)