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

HRID 1380826ノート

反応式

HRID 1380826 の反応式
[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]

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 23324656HCID 23324656、化合物HCID 23699411potassium O-ethyl S-(n-propyl) dithiophosphate

生成物 1

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

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
45 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-65aaff459f064f11b28e2bf9e069b82f
出典データセット
uspto-grants-1986_04
特許番号
US04584295

反応ノート

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