Sodium Iodide → O-ethyl S-(6-ethoxy-2-methyl-4-pyrimidinylmethyl) S-(n-propyl) dithiophosphate

HRID 1380826노트

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HRID 1380826 반응식
[CH2:1]([O:3][C:4]1[N:9]=[C:8]([CH3:10])[N:7]=[C:6]([CH2:11]Cl)[CH:5]=1)[CH3:2].[P:13]([O-:22])([O:19][CH2:20][CH3:21])([S:15][CH2:16][CH2:17][CH3:18])=[S:14].[K+].[I-].[Na+]>CC(C)=O>[P:13]([S:15][CH2:16][CH2:17][CH3:18])([O:19][CH2:20][CH3:21])([S:14][CH2:11][C:6]1[CH:5]=[C:4]([O:3][CH2:1][CH3:2])[N:9]=[C:8]([CH3:10])[N:7]=1)=[O:22]

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 23324656HCID 23324656, 화합물HCID 23699411potassium O-ethyl S-(n-propyl) dithiophosphate

생성물 1

HCID 57315843O-ethyl S-(6-ethoxy-2-methyl-4-pyrimidinylmethyl) S-(n-propyl) dithiophosphate

시약·촉매·용매 1

HCID 180Acetone용매

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온도
45 °C

실험 절차

8.0 g (0.043 mol) of 6-ethoxy-4-chloromethyl-2-methyl-pyrimidine and 10.8 g (0.045 mol) of potassium O-ethyl S-(n-propyl) dithiophosphate are suspended in 20 ml of acetone. After the addition of a small amount (spatula tip) of sodium iodide the mixture is stirred well at 45° C. for 12 hours. The mixture is then filtered through Celite, the filtrate is concentrated under reduced pressure and the thus-isolated solid is taken up in 100 ml of toluene. The toluene solution is washed once with 5% sodium carbonate solution and once with saturated sodium chloride solution and dried over anhydrous sodium sulphate, and the solvent is removed by evaporation at 60° C. under reduced pressure. In this manner there is obtained O-ethyl S-(6-ethoxy-2-methyl-4-pyrimidinylmethyl) S-(n-propyl) dithiophosphate as an almost colourless oil, nD20 1.5385.

후처리

  1. filtrationThe mixture is then filtered through Celite
  2. concentrationthe filtrate is concentrated under reduced pressure
  3. washThe toluene solution is washed once with 5% sodium carbonate solution and once with saturated sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulphate
  5. customthe solvent is removed by evaporation at 60° C. under reduced pressure

출처 및 근거

ORD 기록
ord-65aaff459f064f11b28e2bf9e069b82f
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04584295

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