Sodium hydride → 2-Methylthio-5-diethylphosphonomethylthio-1,3,4-thiadiazole

HRID 354041노트

반응식

HRID 354041 반응식
[CH3:1][S:2][C:3]1[S:4][C:5]([SH:8])=[N:6][N:7]=1.[H-].[Na+].FC(F)(F)S(O[CH2:17][P:18]([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])=[O:19])(=O)=O>C1COCC1>[CH3:1][S:2][C:3]1[S:4][C:5]([S:8][CH2:17][P:18]([O:23][CH2:24][CH3:25])([O:20][CH2:21][CH3:22])=[O:19])=[N:6][N:7]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 11833487(Diethoxyphosphoryl)methyl trifluoromethanesulfonateHCID 1785036205-methylsulfanyl-1,3,4-thiadiazole-2-thiol

생성물 1

HCID 537638322-Methylthio-5-diethylphosphonomethylthio-1,3,4-thiadiazole

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-methylthio-1,3,4-thiadiazole-5-thiol (1 mmole) in THF (5 mL) was treated with sodium hydride (60%, 1.1 mmole) at 0° C. and the resulting mixture was stirred at room temperature for 30 min. The reaction was then cooled to 0° C. and treated with diethylphosphonomethyl trifluoromethanesulfonate (1.1 mmole). After stirring at room temperature for 12 h, the reaction was quenched with saturated ammonium chloride. Extraction and chromatography gave 2-methylthio-5-diethylphosphonomethylthio-1,3,4-thiadiazole as an oil.

후처리

  1. temperatureThe reaction was then cooled to 0° C.
  2. stirringAfter stirring at room temperature for 12 h
  3. customthe reaction was quenched with saturated ammonium chloride
  4. extractionExtraction and chromatography

출처 및 근거

ORD 기록
ord-c2803e40074b4b109f742eebaa47cf1f
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06756360B1

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