Water → HCID 15258078, compound

HRID 1729966

Reaction equation

HRID 1729966 reaction equation
[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]

Participants

7

Reactant 5

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

Product 1

HCID 15258078HCID 15258078, compound

Reagents, catalysts & solvents 1

HCID 6212ChloroformSolvent

Procedure

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.

Workup

  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

Sources & evidence

ORD record
ord-7813ebf51099494993b48c4c0866a009
Source dataset
uspto-grants-1976_11
Patent number
US03991010

Linked notes

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