HRID1371419

反应详情

EQUATION

反应方程式

HRID 1371419 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of Intermediate 9 (0.01 g) in N,N-dimethylformamide (1 ml) was added 1-(chloromethyl)naphthalene (6.1 μl). The mixture was stirred at 22° C. for 24 h before tris-(2-aminoethyl)amine polystyrene (Argonaut Technologies, 0.01 g @ 4.46 mmol/g) and polystyrene methyl isocyanate (Argonaut Technologies, 0.033 g @ 1.39 mmol/g) was added. Stirring was continued for a further 2 h before the mixture was purified by solid phase extraction (Isolute SCX sulphonic acid column), eluting with methanol followed by 10% 0.880 ammonia solution in methanol. The basic fraction was evaporated in vacuo to give the title compound (0.003 g). LC/MS (System A) Rt 2.82 min, Mass Spectrum m/z 4140 [MH+].

WORKUP

后处理

  1. additionwas added
  2. customwas purified by solid phase extraction (Isolute SCX sulphonic acid column)
  3. washeluting with methanol
  4. customThe basic fraction was evaporated in vacuo