Phosphorus oxychloride → HCID 70530187, Verbindung

HRID 647505Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 647505
[C:1]([NH:4][CH2:5][C:6]1[C:11]([CH2:12][CH2:13][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[CH:10][CH:9]=[CH:8][N:7]=1)(=[O:3])[CH3:2].P(Cl)(Cl)([Cl:22])=O>>[OH2:3].[ClH:22].[CH3:2][C:1]1[N:7]2[CH:8]=[CH:9][CH:10]=[C:11]([CH2:12][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]2=[CH:5][N:4]=1.[CH3:2][C:1]1[N:7]2[CH:8]=[CH:9][CH:10]=[C:11]([CH2:12][CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[C:6]2=[CH:5][N:4]=1.[ClH:22]

Komponenten

3

Edukt 2

HCID 24813Phosphorus oxychlorideHCID 20485147N-{[3-(2-Phenylethyl)pyridin-2-yl]methyl}acetamide

Produkt 1

HCID 70530187HCID 70530187, Verbindung

Versuchsvorschrift

Heat a solution of 3.1 gm of the product of Example 8 and 40 ml phosphorous oxychloride at 100° for 20 minutes. Cool to room temperature and remove the phosphorous oxychloride under reduced pressure. Partition the residue between chloroform and an aqueous solution of sodium bicarbonate. Separate the chloroform layer, wash it with brine and dry over potassium carbonate. Filter the dry solution and remove the chloroform under reduced pressure. Dissolve the residue in absolute ethanol and add an ethanolic solution of hydrogen chloride. Remove the ethanol under reduced pressure. Triturate the resulting residue in ether to obtain 3-methyl-8-(2-phenylethyl)imidazo[1,5-a]pyridine hydrochloride hemihydrate as an amorphous, hygroscopic solid.

Aufarbeitung

  1. customremove the phosphorous oxychloride under reduced pressure
  2. customPartition the residue between chloroform
  3. customSeparate the chloroform layer
  4. washwash it with brine
  5. dry with materialdry over potassium carbonate
  6. filtrationFilter the dry solution
  7. customremove the chloroform under reduced pressure
  8. dissolutionDissolve the residue in absolute ethanol
  9. additionadd an ethanolic solution of hydrogen chloride
  10. customRemove the ethanol under reduced pressure
  11. customTriturate the resulting residue in ether

Quellen und Nachweise

ORD-Eintrag
ord-2e8fb9f195424d87adba6f59c6c577a7
Quelldatensatz
uspto-grants-1983_10
Patentnummer
US04409226

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