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

HRID 261674

반응식

HRID 261674 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-3087348359bc4ae9b0c11f2c5b8f51a6
출처 데이터셋
uspto-grants-1979_08
특허 번호
US04166115

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