HCID 14769542、化合物 → HCID 13577105、化合物

HRID 543830ノート

反応式

HRID 543830 の反応式
[CH:1]([NH:3][C:4]1[S:8][N:7]=[C:6]([C:9](=[O:16])[CH:10](SC)[S:11]([CH3:13])=O)[N:5]=1)=[O:2].I([O-])(=O)(=O)=[O:18].[Na+]>C(O)(=O)C>[CH:1]([NH:3][C:4]1[S:8][N:7]=[C:6]([C:9](=[O:16])[C:10]([S:11][CH3:13])=[O:18])[N:5]=1)=[O:2]

参加物

4

反応物 2

HCID 14769542HCID 14769542、化合物HCID 23667635Sodium periodate

生成物 1

HCID 13577105HCID 13577105、化合物収率 129.5%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
70 °C

実験手順

A mixture of 5-formamido-3-(2-methylthio-2-methylsulfinylacetyl)-1,2,4-thiadiazole (0.85 g) and sodium periodate (0.2 g) in glacial acetic acid (10 ml) was stirred for 45 minutes at 70° C. The reaction mixture was evaporated and the residue was dissolved in a mixture of ethyl acetate and water. The mixture was adjusted to pH 7 with an aqueous solution of sodium bicarbonate and treated with an aqueous solution of sodium thiosulfate. The organic layer was separated, dried over anhydrous magnesium sulfate and evaporated to dryness. The residue was triturated with a mixture of diethyl ether and petroleum ether to give the title compound (280 mg), mp. 186° to 187° C.

後処理

  1. customThe reaction mixture was evaporated
  2. dissolutionthe residue was dissolved in a mixture of ethyl acetate and water
  3. additiontreated with an aqueous solution of sodium thiosulfate
  4. customThe organic layer was separated
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customevaporated to dryness
  7. customThe residue was triturated with a mixture of diethyl ether and petroleum ether

出典と根拠

ORDレコード
ord-8eb4b60682de472ca0a2dc32f06869a3
出典データセット
uspto-grants-1984_05
特許番号
US04447429

反応ノート

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