HRID2166312

反应详情

EQUATION

反应方程式

HRID 2166312 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a stirred suspension of chromous chloride (3.3 g) in 75 mL of dry THF was added a solution of iodoform (3.5 g) and N-(4-chlorophenyl)-2,2-dimethyl-3-oxopropanamide (1 g) in 25 mL of THF, dropwise over 10 minutes. The solution was allowed to stir an additional 1.5 hour, then poured into 100 g of ice water and extracted into ether. The organic phase was dried, filtered and evaporated, and the residue was filtered through a small silica gel column, eluting with ether, to remove chromium residues. The title product (0.55 g) was isolated as a solid, m.p. 145°-146° C.

WORKUP

后处理

  1. extractionextracted into ether
  2. customThe organic phase was dried
  3. filtrationfiltered
  4. customevaporated
  5. filtrationthe residue was filtered through a small silica gel column
  6. washeluting with ether
  7. customto remove chromium residues