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Potassium Carbonate → HCID 13277758, 화합물

HRID 2296377
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HRID 2296377 반응식
[CH3:1][CH:2]([C:4]1[N:9]=[CH:8][C:7]([OH:10])=[CH:6][N:5]=1)[CH3:3].C(=O)([O-])[O-].[K+].[K+].[P:17](=[S:25])(Cl)([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20].[H][H]>C(#N)C>[P:17](=[S:25])([O:10][C:7]1[CH:6]=[N:5][C:4]([CH:2]([CH3:3])[CH3:1])=[N:9][CH:8]=1)([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20]
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HCID 11430Potassium CarbonateHCID 17305O,O-diethyl phosphorochloridothioate2회HCID 132777572-(Propan-2-yl)pyrimidin-5-olHCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 13277758HCID 13277758, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile
용매

실험 절차

To a stirred mixture of 166 grams of 2-(1-methylethyl)-5-pyrimidinol, 230 grams of finely powdered potassium carbonate and 1400 ml of acetonitrile was added in a slow stream 226 grams of O,O-diethyl phosphorochloridothioate. The mixture warmed to 55°. Stirring was continued until no more O,O-diethyl phosphorochloridothioate could be detected by GLC. The solids present were removed by filtration, the filtrate concentrated under vacuum, the residue taken up in diethyl ether, the ether solution washed twice with 2% aqueous sodium hydroxide, and once with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The ether was removed under vacuum leaving a pale yellow oil having a refractive index at 25° of 1.4944. On elemental analysis the product was found to contain 45.68% carbon; 6.54% hydrogen and 9.57% nitrogen. Theoretical is 45.50% carbon; 6.60% hydrogen and 9.65% nitrogen.

후처리

  1. temperatureThe mixture warmed to 55°
  2. customThe solids present were removed by filtration
  3. concentrationthe filtrate concentrated under vacuum
  4. washthe ether solution washed twice with 2% aqueous sodium hydroxide
  5. dry with materialonce with saturated sodium chloride solution and dried over anhydrous sodium sulfate
  6. customThe ether was removed under vacuum
  7. customleaving a pale yellow oil
  8. customat 25°

출처 및 근거

ORD 기록
ord-4d6daf6c68df4948bd680cb57729f376
출처 데이터셋
uspto-grants-1984_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04429125

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