Triethyl Phosphate → Potassium diethyl phosphate

HRID 3961

反応式

HRID 3961 の反応式
[CH2:1]([O:3][P:4]([O:9]CC)([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].C[Si](C)(C)[O-].[K+:17]>O1CCCC1>[CH2:1]([O:3][P:4]([O-:9])([O:6][CH2:7][CH3:8])=[O:5])[CH3:2].[K+:17]

参加物

4

反応物 2

HCID 6535Triethyl PhosphateHCID 23668039Potassium trimethylsilanolate

生成物 1

HCID 23663701Potassium diethyl phosphate収率 92.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The procedure of Example 1 was followed except that triethylphosphate (3.4 mL, 20 mmol) was added by syringe to a slurry of potassium trimethylsilanolate (2.56 g, 20 mmol) in dry tetrahydrofuran (50 mL), and a 2 h reaction time at room temperature was used, followed by 40 h of heating at reflux. Potassium diethylphosphate (3.55 g, 92% yield) was isolated as a white solid: 1H NMR (D2O, DSS) δ 1.1 (t, J=6.9 Hz, 6H), 3.75 (q, J=6.9 Hz, 4H). Anal. Calcd. for C4H10KO4P: C, 25.00; H, 5.24; K, 20.34. Found: C, 25.83, 25.88; H, 5.40, 5.29; K, 20.37, 20.10.

後処理

  1. customa 2 h reaction time at room temperature
  2. temperatureof heating
  3. temperatureat reflux

出典と根拠

ORDレコード
ord-71c80b666f9146bca8517cd2a6af9e46
出典データセット
uspto-grants-1988_02
特許番号
US04723016

関連ノート

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