Potassium Carbonate → HCID 13277769、化合物

HRID 2296379ノート

反応式

HRID 2296379 の反応式
[CH2:1]([C:3]1[N:8]=[CH:7][C:6]([OH:9])=[CH:5][N:4]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].[P:16]([S:22][CH2:23][CH:24]([CH3:26])[CH3:25])(=[S:21])(Cl)[O:17][CH2:18][CH3:19].[H][H]>C(#N)C>[P:16]([S:22][CH2:23][CH:24]([CH3:26])[CH3:25])(=[S:21])([O:9][C:6]1[CH:5]=[N:4][C:3]([CH2:1][CH3:2])=[N:8][CH:7]=1)[O:17][CH2:18][CH3:19]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 13079909O-Ethyl S-(2-methylpropyl) phosphorochloridodithioateHCID 136077292-Ethylpyrimidin-5-olHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 13277769HCID 13277769、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 5 grams of 2-ethyl-5-pyrimidinol, 5 grams of finely powdered potassium carbonate, 40 ml of acetonitrile and 9.3 grams of O-ethyl S-(2-methylpropyl) phosphorochloridodithioate was stirred without external heating overnight. The solids were then 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 in a rotary evaporator leaving a pale amber colored oil having a refractive index of 25° of 1.5296. Elemental analysis showed the product contained 44.81% carbon; 6.58% hydrogen and 8.59% nitrogen. Theoretical analysis is 44.98% carbon; 6.61% hydrogen and 8.74% nitrogen.

後処理

  1. temperaturewithout external heating overnight
  2. customThe solids were then 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 in a rotary evaporator
  7. customleaving a pale amber

出典と根拠

ORDレコード
ord-49307633203d45e9ab4f72387e95691e
出典データセット
uspto-grants-1984_01
特許番号
US04429125

反応ノート

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