Water → HCID 15258078、化合物

HRID 1729966

反応式

HRID 1729966 の反応式
[CH:1]([P:3](Cl)(Cl)=[O:4])=[CH2:2].[CH2:7]([OH:10])[CH:8]=[CH2:9].C(N([CH2:16][CH3:17])CC)C.Cl.[CH2:19](N(CC)CC)C.[OH2:26]>C(Cl)(Cl)Cl>[CH2:19]([O:26][P:3]([CH:1]=[CH2:2])(=[O:4])[O:10][CH2:7][CH:8]=[CH2:9])[CH:16]=[CH2:17]

参加物

7

反応物 5

HCID 962WaterHCID 7858Allyl AlcoholHCID 8471TriethylamineHCID 11130Triethylamine hydrochlorideHCID 74035Phosphonic dichloride, ethenyl-

生成物 1

HCID 15258078HCID 15258078、化合物

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

146 g of vinylphosphonic acid dichloride (1 mole) were added while stirring to a solution of 116 g (2 moles) of allyl alcohol in 1000 ml of anhydrous chloroform at 0° C and subsequently 288 g of triethylamine were introduced dropwise within approximately one hour. After suction, the solid residue (triethylamine hydrochloride) was dissolved in water, the oily layer formed was separated and combined with the filtrate. The filtrate was extracted four times with 600 ml of water each time in order to remove the chlorine, dried over sodium sulfate and the chloroform was distilled off in the rotation evaporator. 190 g of a brown liquid were obtained, having a boiling point of from 75° to 80° C at 5 mm Hg.

後処理

  1. customthe oily layer formed
  2. customwas separated
  3. extractionThe filtrate was extracted four times with 600 ml of water each time in order
  4. customto remove the chlorine
  5. dry with materialdried over sodium sulfate
  6. distillationthe chloroform was distilled off in the rotation evaporator

出典と根拠

ORDレコード
ord-7813ebf51099494993b48c4c0866a009
出典データセット
uspto-grants-1976_11
特許番号
US03991010

関連ノート

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