3-(Piperazin-1-yl)propane-1,2-diol → 3-[4-(4-Cyanopyridazin-3-yl)piperazin-1yl]propane-1,2-diol dihydrochloride

HRID 231771Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 231771
[OH:1][CH:2]([CH2:10][OH:11])[CH2:3][N:4]1[CH2:9][CH2:8][NH:7][CH2:6][CH2:5]1.[C:12]([C:14]1[CH:19]=[CH:18][N:17]=[N:16][C:15]=1[Cl:20])#[N:13]>O1CCOCC1.Cl.C(O)(C)C>[ClH:20].[ClH:20].[C:12]([C:14]1[CH:19]=[CH:18][N:17]=[N:16][C:15]=1[N:7]1[CH2:8][CH2:9][N:4]([CH2:3][CH:2]([OH:1])[CH2:10][OH:11])[CH2:5][CH2:6]1)#[N:13]

Komponenten

6

Edukt 2

HCID 1110023-(Piperazin-1-yl)propane-1,2-diolHCID 123709723-Chloropyridazine-4-carbonitrile

Produkt 1

HCID 200320153-[4-(4-Cyanopyridazin-3-yl)piperazin-1yl]propane-1,2-diol dihydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 313Hydrochloric AcidLösungsmittelHCID 3776IsopropanolLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Grams 6.9 of 1-(2,3-dihydroxypropyl)piperazine and 3.0 g of 4-cyano-3-chloropyridazine in 60 ml dioxane were refluxed for 2 hours. The reaction mixture was settled, the supernatant liquor evaporated to dryness and the residue, which formed, was dissolved in 10 ml concentrated hydrochloric acid and diluted with 10 volumes of isopropanol. A precipitate was obtained formed by a gummy oil, which solidified afterwards giving 5.9 g of 3-[4-(4-cyanopyridazin-3-yl)piperazin-1yl]propane-1,2-diol dihydrochloride which melted at 128°-130° C.

Aufarbeitung

  1. customthe supernatant liquor evaporated to dryness
  2. customthe residue, which formed
  3. customA precipitate was obtained
  4. customformed by a gummy oil, which

Quellen und Nachweise

ORD-Eintrag
ord-f2986ccf2e044ec0b57fdf96135df790
Quelldatensatz
uspto-grants-1989_07
Patentnummer
US04849422

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