HRID660712

反应详情

EQUATION

反应方程式

HRID 660712 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A mixture of 5-(2-benzyloxy-4-iodophenyl)-1,1-dioxo-1,2,5-thiadiazolidin-3-one (200 mg, 0.45 mmol), trans-1-hexen-1-ylboronic acid (77 mg, 0.676 mmol), resin-bound PPh3Pd (692 mg, loading 0.13 mmol/g) and aqueous Na2CO3 (0.9 mL of a 2M solution) in DME (3 mL) is placed in a microwave vial and heated at 110° C. for 30 min. The mixture is filtered, diluted with EtOAc and washed with 1N HCl. The organic phase is dried over magnesium sulfate and the solvent removed under reduced pressure. The residue is purified by preparative HPLC to give the title compound.

WORKUP

后处理

  1. filtrationThe mixture is filtered
  2. additiondiluted with EtOAc
  3. washwashed with 1N HCl
  4. dry with materialThe organic phase is dried over magnesium sulfate
  5. customthe solvent removed under reduced pressure
  6. customThe residue is purified by preparative HPLC