HCID 14769542, 화합물 → HCID 13577105, 화합물

HRID 1381344노트

반응식

HRID 1381344 반응식
[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]

참가 물질

4

반응물 2

HCID 14769542HCID 14769542, 화합물HCID 23667635Sodium periodate

생성물 1

HCID 13577105HCID 13577105, 화합물수율 129.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ddd3423ee5574c34ab9822c9024bf301
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04585872

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