HRID1948278

反应详情

EQUATION

反应方程式

HRID 1948278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

According to Scheme 33 Step 1: 1-((6-Chloropyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (2.54 mmol, 0.83 g), trimethylsilyl chloride (3.3 mmol, 0.42 mL) and NaI (7.60 mmol, 1.14 g) in propionitrile (20 mL) were heated at 140° C. for 20 minutes under microwave irradiation conditions. Then the suspension was filtered off and the solid obtained was partitioned between CH2Cl2/water. The aqueous layer was extracted several times with CH2Cl2; the organic layers were combined, dried (Na2SO4) and the solvent was evaporated under reduced pressure. The residue was treated with Et2O giving an 1-((6-iodopyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (600 mg, 61%) as a pale grey solid.

WORKUP

后处理

  1. filtrationThen the suspension was filtered off
  2. customthe solid obtained
  3. customwas partitioned between CH2Cl2/water
  4. extractionThe aqueous layer was extracted several times with CH2Cl2
  5. dry with materialdried (Na2SO4)
  6. customthe solvent was evaporated under reduced pressure
  7. additionThe residue was treated with Et2O giving an 1-((6-iodopyridin-3-yl)methyl)-5-(4-methoxyphenyl)pyridin-2(1H)-one (600 mg, 61%) as a pale grey solid