Ethylene → Phosphinic acid, P,P-diethyl-, aluminum salt (3:1)

HRID 1868566

反応式

HRID 1868566 の反応式
O.[PH2:2]([O-:4])=[O:3].[Na+].[CH2:6]=[CH2:7].[C:8](OOC(=O)[C:19]1[CH:24]=CC=CC=1)(=O)[C:9]1C=CC=CC=1.O.O.O.O.O.O.O.O.O.[N+]([O-])([O-])=O.[Al+3:39].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>O>[CH2:8]([P:2]([CH2:6][CH3:7])(=[O:4])[O-:3])[CH3:9].[Al+3:39].[CH2:6]([P:2]([CH2:24][CH3:19])(=[O:4])[O-:3])[CH3:7].[CH2:8]([P:2]([CH2:6][CH3:7])(=[O:4])[O-:3])[CH3:9]

参加物

6

反応物 4

HCID 6325Ethylene2 回HCID 7187Benzoyl PeroxideHCID 24567Aluminum nitrate nonahydrateHCID 178418950HCID 178418950、化合物

生成物 1

HCID 21863131Phosphinic acid, P,P-diethyl-, aluminum salt (3:1)

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

反応条件

温度
100 °C

実験手順

1500 g (14 mol) of sodium hypophosphite monohydrate were dissolved in 7.5 kg of water and used as initial charge in a 16 l jacketed pressure reactor composed of enameled steel. Once the reaction mixture had been heated to 100° C., ethylene was introduced by way of a reducing valve set to 6 bar until saturation had been reached in the reactor. A solution of 49 g (1 mol %) of dibenzoyl peroxide (70% by weight in water) in 300 g of water was uniformly metered in over a period of 6 h with constant stirring, at an ethylene pressure of 6 bar and a temperature of from 100 to 110° C. After a continued reaction time of 1 h, depressurization of the reactor, and cooling to about 90° C., 1725 g (4.67 mol of aluminum) of aluminum nitrate nonahydrate dissolved in 1275 g of water were added over a period of 60 min. The resultant solid was then filtered off, washed with 2 l of hot water and vacuum-dried at 130° C. Yield: 1697 g (92.2% of theory).

後処理

  1. additionas initial charge in a 16 l jacketed pressure reactor
  2. customof from 100 to 110° C
  3. temperatureAfter a continued reaction time of 1 h, depressurization of the reactor, and cooling to about 90° C.
  4. additionwere added over a period of 60 min
  5. filtrationThe resultant solid was then filtered off
  6. washwashed with 2 l of hot water
  7. customvacuum-dried at 130° C

出典と根拠

ORDレコード
ord-30db3cbf43aa4344bd13fbb9b504c589
出典データセット
uspto-grants-2009_12
特許番号
US07635785B2

関連ノート

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