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

HRID 231771ノート

反応式

HRID 231771 の反応式
[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]

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 3776Isopropanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f2986ccf2e044ec0b57fdf96135df790
出典データセット
uspto-grants-1989_07
特許番号
US04849422

反応ノート

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