反应详情

温度

25 °C

A 1 M solution of Br2 in DMF (12.9 mL, 13.2 mmol) is added dropwise to a solution of (4-methoxy-phenyl)-thiazol-2-yl-amine (2.72 g, 13.2 mmol) in DMF (40 mL), under an argon atmosphere. During the addition, the internal temperature of the reaction mixture is kept below 26° C. The mixture is stirred for 20 min at 25° C. and concentrated in vacuo. Purification of the crude product by silica gel (250 g) column chromatography (CH2Cl2/MeOH, 99/1) affords the title compound: ES-MS: 287.0 [M+H]+; single peak at tR=7.99 min (System 1); Rf=0.47 (CH2Cl2/MeOH, 98/2).

1. additionDuring the addition
2. customis kept below 26° C
3. concentrationconcentrated in vacuo
4. customPurification of the crude product by silica gel (250 g) column chromatography (CH2Cl2/MeOH, 99/1)