反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a similar manner to Example 1, t-butyl 4-[3-(6-thiocarbamoylpyrid-3-ylcarbonyl)ureido]phenoxyacetate (2.73 g) was reacted with iodomethane (13 ml) and acetone (200 ml) and the resultant product was treated with ammonium acetate (6 g), methanol (30 ml) and dichloromethane (30 ml) at ambient temperature. This yielded a crude solid which was collected and washed with methanol and acetone to give the title compound (1.68 g) as an orange solid: m.p. 290°-300° C. (decomposes); NMR Spectrum (DMSO-d6) 1.43 (9H, s), 1.82 (3H, s), 4.62 (2H, s), 6.90 (2H, d), 7.49 (2H, d), 8.29 (1H, d), 8.52 (1H, dd), 9.18 (1H, d) 10.61 (1H, s); Mass Spectrum m/Z 414 (M+H)+ ; Elemental Analysis: calculated for C20H23N5O5. 1.0 CH3CO2H. 0.5 H2O: C, 54.8%; H, 5.85%; N, 14.5%; found: C, 54.6%; H, 6.0%; N, 14.5%
WORKUP
后处理
- customThis yielded a crude solid which
- customwas collected
- washwashed with methanol and acetone