HRID970623
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of Compound 107 (1 g, 2.64 mmol), 4-(2-chloro ethyl) morpholine (2.45 g, 13.2 mmol), and potassium carbonate (3.64 g, 26.4 mmol) in DMF was heated overnight at 90° C. The solution was cooled and poured into ice water. The solids formed were filtered, washed by water, and dried. The crude product was purified by flash chromatography eluting with 0-110% methanol in ethylacetate gradient to yield 223 mg (17%) of white solids. M.P. 207° C. 1H NMR (DMSO-d6): δ 2.40 (s, 3H), 3.54 (m, 4H), 3.63 (m, 4H), 3.92 (m, 4H), 4.35 (m, 2H), 7.16 (dd, J=3.4, 4.8 Hz, 1H), 7.49 (m, 2H), 7.61 (m, 1H), 7.69 (s, 1H), 7.80 (d, J=5.2 Hz, 1H). EIMS m/z 492 (M+1). Anal. (C26H29N5O3S) C, H, N.
WORKUP
后处理
- temperatureThe solution was cooled
- customThe solids formed
- filtrationwere filtered
- washwashed by water
- customdried
- customThe crude product was purified by flash chromatography
- washeluting with 0-110% methanol in ethylacetate gradient