6-(4,4-Ethylenedioxy-1-piperidinyl)-8-methyl-1,2,4-triazolo [4,3-b]pyridazine → 1-(8-Methyl-1,2,4-triazolo [4,3-b]pyridazin-6-yl)-4-piperidinone

HRID 1492398ノート

反応式

HRID 1492398 の反応式
C1CO[C:3]2([CH2:8][CH2:7][N:6]([C:9]3[CH:10]=[C:11]([CH3:18])[C:12]4[N:13]([CH:15]=[N:16][N:17]=4)[N:14]=3)[CH2:5][CH2:4]2)[O:2]1>C(O)(=O)C>[CH3:18][C:11]1[C:12]2[N:13]([CH:15]=[N:16][N:17]=2)[N:14]=[C:9]([N:6]2[CH2:7][CH2:8][C:3](=[O:2])[CH2:4][CH2:5]2)[CH:10]=1

参加物

3

反応物 1

HCID 232003096-(4,4-Ethylenedioxy-1-piperidinyl)-8-methyl-1,2,4-triazolo [4,3-b]pyridazine

生成物 1

HCID 189505491-(8-Methyl-1,2,4-triazolo [4,3-b]pyridazin-6-yl)-4-piperidinone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A solution of 62.5 g of 6-(4,4-ethylenedioxy-1-piperidinyl)-8-methyl-1,2,4-triazolo [4,3-b]pyridazine in 350 ml of aqueous 10% acetic acid was refluxed for 7 hours. The solvent was then evaporated under reduced pressure and the residue was taken up in 1100 ml of boiling ethanol. The ethanol solution was concentrated to 600 ml and cooled in an ice bath. The crystalline solid which formed was separated by filtration, washed with fresh ethanol and then with ethyl ether and dried to give 1-(8-methyl-1,2,4-triazolo [4,3-b]pyridazin-6-yl)-4-piperidinone as cream-colored needles melting at about 196.5°-199° C.

後処理

  1. customThe solvent was then evaporated under reduced pressure
  2. concentrationThe ethanol solution was concentrated to 600 ml
  3. temperaturecooled in an ice bath
  4. customThe crystalline solid which formed
  5. customwas separated by filtration
  6. washwashed with fresh ethanol
  7. dry with materialwith ethyl ether and dried

出典と根拠

ORDレコード
ord-63c8a031fbde412ebb1d824d5e552662
出典データセット
uspto-grants-1994_12
特許番号
US05374632

反応ノート

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