Pyridine → HCID 53712289、化合物

HRID 441692

反応式

HRID 441692 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: Analysis: C8H14ClO3P Mol weight: 224.6

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-aa0b7fa6007743a9833061d13c2e218a
出典データセット
uspto-grants-1977_08
特許番号
US04042370

関連ノート

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