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

HRID 325372

反応式

HRID 325372 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].C>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

7

反応物 5

HCID 297MethaneHCID 24007Selenium DioxideHCID 312751,4-DioxaneHCID 3145078Ethyl 2-methanesulfonamidothiazol-4-ylacetateHCID 178470766HCID 178470766、化合物

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

To a solution prepared by stirring a mixture of selenium dioxide (0.22 g.), dioxane (10 ml.) and water (0.2 ml.) for 10 minutes at 110° C. was added ethyl 2-(2-mesylamino-1,3-thiazol-4-yl)acetate, which can be represented as ethyl 2-(2-mesylimino-2,3-dihydro-1,3-thiazol-4-yl)acetate, (0.53 g.), and the mixture was refluxed for 1 hour. After the reaction, the reaction mixture was treated with activated charcoal. The precipitated crystals in the filtrate were collected by filtration and dried to give white crystals of ethyl 2-(2-mesylamino-1,3-thiazol-4-yl)glyoxylate, which can be represented as ethyl 2-(2-mesylimino-2,3-dihydro-1,3-thiazol-4-yl)glyoxylate, (0.22 g.), mp. 222° to 225° C. On the other hand, the remaining filtrate was concentrated and the residue was washed with water and diethyl ether in turn and then dried to give the same object compound (0.12 g.)

後処理

  1. customTo a solution prepared
  2. temperaturethe mixture was refluxed for 1 hour
  3. customAfter the reaction
  4. filtrationThe precipitated crystals in the filtrate were collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-adcb69aaf3b94f7699dde3a0838c2a65
出典データセット
uspto-grants-1984_04
特許番号
US04440766

関連ノート

読み込み中…