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Potassium Iodide → O-[2-(N-cyclopropylcarbamoyloxy)-2-ethoxyiminoethyl] 2-methylphenyl(4-bromophenyl)thionophosphinate

HRID 1578595
ノート
印刷プレビュー

反応式

HRID 1578595 の反応式
Cl[CH2:2][C:3]([O:8][C:9](=[O:14])[NH:10][CH:11]1[CH2:13][CH2:12]1)=[N:4][O:5][CH2:6][CH3:7].[CH3:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[S:22]([C:26]1[CH:31]=[CH:30][C:29]([Br:32])=[CH:28][CH:27]=1)=[P:23](=[O:25])[O-:24].[K+].[I-].[K+]>C(C(C)=O)C>[CH3:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[S:22]([C:26]1[CH:31]=[CH:30][C:29]([Br:32])=[CH:28][CH:27]=1)=[P:23](=[O:24])[O:25][CH2:2][C:3]([O:8][C:9](=[O:14])[NH:10][CH:11]1[CH2:13][CH2:12]1)=[N:4][O:5][CH2:6][CH3:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 4875Potassium IodideHCID 543801311-chloro-2-(N-cyclopropylcarbamoyloxy)-2-ethoxyiminoethaneHCID 131710027Potassium 2-methylphenyl(4-bromophenyl)thionophosphinate

生成物 1

HCID 131710026O-[2-(N-cyclopropylcarbamoyloxy)-2-ethoxyiminoethyl] 2-methylphenyl(4-bromophenyl)thionophosphinate

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

1-Chloro-2-(N-cyclopropylcarbamoyloxy)-2-ethoxyiminoethane (11 grams; 0.05 mole), methyl ethyl ketone (80 ml), potassium 2-methylphenyl(4-bromophenyl)thionophosphinate (17 grams; 0.05 mole) and a few crystals of potassium iodide are charged into a glass reaction flask equipped with a mechanical stirrer, thermometer and reflux condenser. The reaction mixture is then heated at reflux for a period of about 8 hours. After this time the reaction mixture is cooled to room temperature and is filtered to remove inorganic salts. The salts are washed with acetone and the washings combined with the filtrate. The resulting solution is stripped of solvents in a rotary evaporator. The remaining residue is dissolved in ether and the ether solution is washed with water and dried over anhydrous magnesium sulfate. The dried solution is filtered and stripped of ether to yield the desired product O-[2-(N-cyclopropylcarbamoyloxy)-2-ethoxyiminoethyl] 2-methylphenyl(4-bromophenyl)thionophosphinate.

後処理

  1. customequipped with a mechanical stirrer
  2. temperaturethermometer and reflux condenser
  3. temperatureThe reaction mixture is then heated
  4. temperatureat reflux for a period of about 8 hours
  5. filtrationis filtered
  6. customto remove inorganic salts
  7. washThe salts are washed with acetone
  8. customThe resulting solution is stripped of solvents in a rotary evaporator
  9. dissolutionThe remaining residue is dissolved in ether
  10. washthe ether solution is washed with water
  11. dry with materialdried over anhydrous magnesium sulfate
  12. filtrationThe dried solution is filtered

出典と根拠

ORDレコード
ord-830f603568f34fc589cc0d95b0dd9c6f
出典データセット
uspto-grants-1976_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03937824

反応ノート

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