HRID1166770

反应详情

EQUATION

反应方程式

HRID 1166770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

This compound was prepared analogously to the compound described in the previous example starting from resin bound 3-chloro-4-hydroxybenzoic acid hydrazide (resin—[building block 1]) (2 g, ˜2 mmoles), 4-(2-bromoethoxy)-2-methoxybenzaldehyde ([building block 2]) (0.73 g, 1.5 equivs.), and 1-benzylpiperazine ([building block 3]) (3.3 g, 10 equivs.). After cleavage with 50% trifluoroacetic acid, the residue (1.4 g) was dissolved in 2-propanol (50 ml) and concentrated to 20 ml. The mixture was allowed to stand at 5° C. for 1 h and filtered. The mother liquor was concentrated in vacuo and the residue was purified by column chromatography on silica gel (20 g) eluting with a mixture of methanol and dichloromethane (1:9). This afforded 0.98 g of the title compound.

WORKUP

后处理

  1. customThis compound was prepared analogously to the compound
  2. concentrationconcentrated to 20 ml
  3. filtrationfiltered
  4. concentrationThe mother liquor was concentrated in vacuo
  5. customthe residue was purified by column chromatography on silica gel (20 g)
  6. washeluting with a mixture of methanol and dichloromethane (1:9)