反应详情

About 0.05 g of N-(6-cyano-1,3-benzothiazol-2-yl)-N′-ethylurea was charged into about 10 mL of ethyleneglycol dimethylether. Introduced about 50 mg lithium aluminum hydride in several portions over about 12–24 hours. The slurry was quenched with about 5–10 mL ethyl acetate then about 1–2 mL of saturated aqueous sodium sulfate. The slurry was then diluted with water and extracted with ethyl acetate. Following drying and removal of solvents under reduced pressure, the product was isolated by preparative HPLC. 1H NMR 1.08 (t, 3H), 1.88 (s, 3H), 3.17 (m, 2H), 3.83 (s, 2H), 7.07 (m, 1H), 7.32 (m, 1H), 7.54 (d, 1H), 7.8 (s, 1H); LC/MS 1.86 min, 251 (M+1), 249 (M−1).

1. customThe slurry was quenched with about 5–10 mL ethyl acetate
2. additionThe slurry was then diluted with water
3. extractionextracted with ethyl acetate
4. customFollowing drying
5. customremoval of solvents under reduced pressure
6. customthe product was isolated by preparative HPLC
7. customLC/MS 1.86 min, 251 (M+1), 249 (M−1)