반응 #49026

반응 방정식

4-aminooxy-N-methyl-butylamide

2-fluoro-4-iodophenylamino-5-formyl-N-(2-hydroxy-ethoxy)-benzamide

3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-5-formyl-N-(2-hydroxy-ethoxy)-benzamide

tetrahydrofuran methanol

→

(E)-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-[(3-methylcarbamoyl-propoxyimino)-methyl]-benzamide

수율 79.0%

반응 조건

후처리

1. 1
   농축The reaction mixture was concentrated under reduced pressure to an extent where a little solvent
2. 2
   workup.ADDITIONacetonitrile was added
3. 3
   기타to precipitate the product
4. 4
   여과This precipitate was filtered
5. 5
   세척washed with acetonitrile
6. 6
   기타dried under reduced pressure

실험 절차

To 4-aminooxy-N-methyl-butylamide (1.79 g, 13.54 mmol) obtained in Step B were added a mixed solvent of tetrahydrofuran/methanol (3:1, 100 ml) and 3,4-difluoro-2-(2-fluoro-4-iodophenylamino-5-formyl-N-(2-hydroxy-ethoxy)-benzamide (5.00 g, 10.41 mmol) obtained in Step F of Example 1, and the mixture was stirred for 13 hours. The reaction mixture was concentrated under reduced pressure to an extent where a little solvent remained, and acetonitrile was added thereto to precipitate the product. This precipitate was filtered, washed with acetonitrile, and dried under reduced pressure to give (E)-3,4-difluoro-2-(2-fluoro-4-iodo-phenylamino)-N-(2-hydroxy-ethoxy)-5-[(3-methylcarbamoyl-propoxyimino)-methyl]-benzamide (4.93 g, 79% yield).

출처