Pyridine → HCID 53712289、化合物

HRID 1449303

反応式

HRID 1449303 の反応式
[CH2:1]([OH:4])[CH:2]=[CH2:3].[Cl:5][CH2:6][CH2:7][P:8](Cl)(Cl)=[O:9].N1C=C[CH:15]=[CH:14][CH:13]=1.CC[O:20]CC>>[Cl:5][CH2:6][CH2:7][P:8]([O:9][CH2:13][CH:14]=[CH2:15])(=[O:20])[O:4][CH2:1][CH:2]=[CH2:3]

参加物

5

反応物 4

HCID 1049PyridineHCID 3283Diethyl EtherHCID 7858Allyl AlcoholHCID 69645(2-Chloroethyl)phosphonic dichloride

生成物 1

HCID 53712289HCID 53712289、化合物

実験手順

To a solution of 11.6 g (0.2 mol) of allyl alcohol and 18.1 g (0.1 mol) of 2-chloroethane phosphonic acid dichloride in 150 ml of absolute ether are added dropwise with stirring 15.8 g (0.2 mol) of pyridine. When the exothermic reaction is complete, stirring is continued for 15 hours at 40° after which the precipitated hydrochloride is removed by filtration and the ethereal filtrate washed to neutrality with water, dried and then evaporated. It is further dried by rotation under high vacuum over a period of 2 hours at 25°. A yellowish oil is obtained having the following characterisation data:

後処理

  1. customWhen the exothermic reaction
  2. customafter which the precipitated hydrochloride is removed by filtration
  3. washthe ethereal filtrate washed
  4. customdried
  5. customevaporated
  6. customIt is further dried by rotation under high vacuum over a period of 2 hours at 25°
  7. customA yellowish oil is obtained

出典と根拠

ORDレコード
ord-7d5075e086984f5ca39ac3210093084f
出典データセット
uspto-grants-1980_02
特許番号
US04190430

関連ノート

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