Water → HCID 19612597、化合物

HRID 581014

反応式

HRID 581014 の反応式
[CH2:1]([S:3][CH2:4][CH2:5][OH:6])[CH3:2].C(SCC[O:12][C:13]1[C:14]([C:18]2[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=2)=[N:15][S:16][N:17]=1)C.[CH3:24]S(O)(=O)=O.[OH-:29].[Na+].[OH2:31]>>[C:5]([OH:6])(=[O:12])[C:4]([OH:31])=[O:29].[CH3:24][N:20]1[CH2:21][CH2:22][CH:23]=[C:18]([C:14]2[C:13]([O:29][CH2:2][CH2:1][S:3]([CH2:4][CH3:5])=[O:31])=[N:17][S:16][N:15]=2)[CH2:19]1

参加物

6

反応物 5

HCID 962WaterHCID 6395Methanesulfonic AcidHCID 80752-(Ethylthio)ethanolHCID 14798Sodium HydroxideHCID 19612583HCID 19612583、化合物

生成物 1

HCID 19612597HCID 19612597、化合物

実験手順

1,2,5,6-tetrahydro-1-methyl-3-(3-(2-ethylsulfinyl-1-ethoxy)-1,2,5-thiadiazol-4-yl)pyridine oxalate was prepared in the same manner using 2-(ethylthio)ethanol as the starting alcohol. The intermediate 3-(4-(2-ethylthio-1-ethoxy)-1,2,5-thiadiazol-3-yl)pyridine was oxidized with 1.1 equivalent of NaIO4 and 1 equivalent MeSO3H using water as the reaction solvent. After a reaction time of 3.5 h. the solution was made basic with 2N NaOH and extracted with ethyl acetate. The combined extracts were dried over MgSO4 and evaporated under vacuum. The resulting sulfoxide was then converted to the title compound in the same manner described above. M.p. 171-172° C., M+ : 302. Compound 45.

後処理

  1. customAfter a reaction time of 3.5 h.
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined extracts were dried over MgSO4
  4. customevaporated under vacuum

出典と根拠

ORDレコード
ord-f4b49c8d25fd48f18ca38cf429238176
出典データセット
uspto-grants-1999_07
特許番号
US05919805

関連ノート

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