Potassium Carbonate → O,O-dimethyl O-(2-(1,1-dimethylethyl)-5-pyrimidinyl) phosphorothioate

HRID 568769

반응식

HRID 568769 반응식
[CH3:1][C:2]([C:5]1[N:10]=[CH:9][C:8]([OH:11])=[CH:7][N:6]=1)([CH3:4])[CH3:3].C(=O)([O-])[O-].[K+].[K+].[P:18](=[S:24])(Cl)([O:21][CH3:22])[O:19][CH3:20].[H][H]>C(#N)C>[P:18](=[S:24])([O:11][C:8]1[CH:7]=[N:6][C:5]([C:2]([CH3:1])([CH3:3])[CH3:4])=[N:10][CH:9]=1)([O:21][CH3:22])[O:19][CH3:20]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 17304Dimethyl phosphorochloridothionate2회HCID 1634995-Pyrimidinol, 2-(1,1-dimethylethyl)-HCID 178418361HCID 178418361, 화합물2회

생성물 1

HCID 13277768O,O-dimethyl O-(2-(1,1-dimethylethyl)-5-pyrimidinyl) phosphorothioate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a stirred mixture of 6 grams of 2-(1,1-dimethylethyl)-5-pyrimidinol, 6 grams of finely powdered potassium carbonate and 40 ml of acetonitrile was added 6.33 grams of O,O-dimethyl phosphorochloridothioate. The mixture was stirred without external heating until all O,O-dimethyl phosphorochloridothioate was consumed as shown 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, once with saturated sodium chloride solution and dried over anhydrous sodium sulfate. The solvent was removed under vacuum, while leaving a pale amber colored oil having a refractive index at 25° of 1.5027. Elemental analysis showed the product to contain 43.82% carbon; 6.09% hydrogen and 10.10% nitrogen. Theoretical composition is 43.47% carbon; 6.20% hydrogen and 10.14% nitrogen.

후처리

  1. customwas consumed
  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, once with saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. customThe solvent was removed under vacuum
  7. customwhile leaving a pale amber
  8. customat 25°

출처 및 근거

ORD 기록
ord-d5712e2a5fba4062ab935c247c7f8137
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04729987

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