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

HRID 231771노트

반응식

HRID 231771 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 3776Isopropanol용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-f2986ccf2e044ec0b57fdf96135df790
출처 데이터셋
uspto-grants-1989_07
특허 번호
US04849422

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