Water → HCID 19612597, 화합물

HRID 1600312

반응식

HRID 1600312 반응식
[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

참가 물질

6

반응물 5

HCID 962WaterHCID 6395Methanesulfonic AcidHCID 80752-(Ethylthio)ethanolHCID 14798Sodium HydroxideHCID 196125833-(4-(2-Ethylthio-1-ethoxy)-1,2,5-thiadiazol-3-yl)pyridine

생성물 1

HCID 19612597HCID 19612597, 화합물

실험 절차

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 NalO4 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. Thecombined 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 112.

후처리

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

출처 및 근거

ORD 기록
ord-dc415f9d95544fe286ee7a9746abe573
출처 데이터셋
uspto-grants-1998_04
특허 번호
US05744489

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