Selenium Dioxide → Ethyl 2-(2-mesylamino-1,3-thiazol-4-yl)glyoxylate

HRID 463852

反応式

HRID 463852 の反応式
[Se](=O)=O.[O:4]1CCOCC1.[S:10]([NH:14][C:15]1[S:16][CH:17]=[C:18]([CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22])[N:19]=1)([CH3:13])(=[O:12])=[O:11]>O>[S:10]([NH:14][C:15]1[S:16][CH:17]=[C:18]([C:20](=[O:4])[C:21]([O:23][CH2:24][CH3:25])=[O:22])[N:19]=1)([CH3:13])(=[O:11])=[O:12]

参加物

5

反応物 3

HCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 3145078Ethyl 2-methanesulfonamidothiazol-4-ylacetate

生成物 1

HCID 19978726Ethyl 2-(2-mesylamino-1,3-thiazol-4-yl)glyoxylate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of selenium dioxide (11.1 g.), dioxane (250 ml.) and water (5 ml.) was stirred for 15 minutes at 110° to 115° C. to give yellow solution. Ethyl 2-(2-mesylamino-1,3-thiazol-4-yl)acetate (26.4 g) was added thereto with stirring at the same temperature. After stirring for 1 hour, the reaction mixture was decanted with heating and cooled to precipitate yellow crystals. The crystals were collected by filtration, washed with dioxane and ether and dried to give ethyl 2-(2-mesylamino-1,3-thiazol-4-yl)glyoxylate (23.5 g.).

後処理

  1. customto give yellow solution
  2. stirringwith stirring at the same temperature
  3. stirringAfter stirring for 1 hour
  4. customthe reaction mixture was decanted
  5. temperaturewith heating
  6. temperaturecooled
  7. customto precipitate yellow crystals
  8. filtrationThe crystals were collected by filtration
  9. washwashed with dioxane and ether
  10. customdried

出典と根拠

ORDレコード
ord-d1da65eadd1c4c1196592e17b12e83d8
出典データセット
uspto-grants-1985_10
特許番号
US04544653

関連ノート

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