Methane → HCID 21436923, compound

HRID 2397173Notes

Reaction equation

HRID 2397173 reaction equation
S(Cl)([Cl:3])=O.[Cl-:5].[CH3:6][P+:7]1([CH2:12][CH2:13]O)[CH2:11][CH2:10][CH2:9][CH2:8]1.Cl.C>C(Cl)(Cl)Cl.CN(C)C=O>[Cl-:3].[CH3:6][P+:7]1([CH2:12][CH2:13][Cl:5])[CH2:11][CH2:10][CH2:9][CH2:8]1

Participants

7

Reactant 4

HCID 297MethaneHCID 313Hydrochloric AcidHCID 24386Thionyl ChlorideHCID 21436928HCID 21436928, compound

Product 1

HCID 21436923HCID 21436923, compound

Reagents, catalysts & solvents 2

HCID 6212ChloroformSolventHCID 6228DimethylformamideSolvent

Procedure

27.3 g (0.23 mole) of thionyl chloride were added dropwise, whilst stirring, to a solution of 36.5 g (0.2 mole) of 1-methyl-1(2-hydroxyethyl)-phospholanium chloride in 200 ml of chloroform and a small amount of dimethylformamide at 65° C. When the evolution of hydrogen chloride had subsided, the reaction mixture was concentrated under reduced pressure and the residue which remained was taken up in water. The solution thereby produced was treated with active charcoal and then filtered. Concentration of the filtrate under reduced pressure gave 1-methyl-1-(2-chloroethyl)-phospholanium chloride in the form of a crystal hydrate from which water was eliminated on warming at 70° C. The substance which remained melted above 250° C.

Workup

  1. customat 65° C
  2. concentrationthe reaction mixture was concentrated under reduced pressure
  3. customThe solution thereby produced
  4. filtrationfiltered

Sources & evidence

ORD record
ord-43747b2801a34c68ad7d02ccec0ddc24
Source dataset
uspto-grants-1977_05
Patent number
US04021221

Reaction notes

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