HRID1900879

反应详情

EQUATION

反应方程式

HRID 1900879 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. customThis yielded a crude solid which
  2. customwas collected
  3. washwashed with methanol and acetone