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Diethyl Ether → HCID 178486115, 화합물

HRID 1578997
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HRID 1578997 반응식
[Cl-].[CH3:2][N:3]([S+:5]([N:9]([CH3:11])[CH3:10])[N:6]([CH3:8])[CH3:7])[CH3:4].[O-:12][C:13]#[N:14].[Na+].CCOCC>CO>[O-:12][C:13]#[N:14].[CH3:2][N:3]([S+:5]([N:9]([CH3:11])[CH3:10])[N:6]([CH3:8])[CH3:7])[CH3:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 517096Sodium CyanateHCID 86733077HCID 86733077, 화합물

생성물 1

HCID 178486115HCID 178486115, 화합물수율 90%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 10 g (0.05 mole) of tris(dimethylamino)sulfonium chloride and 3.6 g (0.055 mole) powdered sodium cyanate in 100 ml methanol was stirred at room temperature (25°) for 3 days. Ether, 300 ml, was added, and the precipitated sodium chloride was filtered off. The filtrate was evaporated to dryness under reduced pressure and the residue was redissolved in acetonitrile, filtered, and then precipitated by the addition of ether. The precipitate was collected on a filter, washed with ether, and dried under dry nitrogen to give 9.27 g (90%) of tris(dimethylamino)sulfonium cyanate as a white crystalline powder, m.p. 202°-204°.

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후처리

  1. filtrationthe precipitated sodium chloride was filtered off
  2. customThe filtrate was evaporated to dryness under reduced pressure
  3. dissolutionthe residue was redissolved in acetonitrile
  4. filtrationfiltered
  5. customprecipitated by the addition of ether
  6. customThe precipitate was collected on a filter
  7. washwashed with ether
  8. customdried under dry nitrogen

출처 및 근거

ORD 기록
ord-7cee66f468644d9985726c8e44ebeb95
출처 데이터셋
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03940402

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