3,6-Octanedione → HCID 23275890、化合物

HRID 1389998ノート

反応式

HRID 1389998 の反応式
[NH:1]([C:3]1[N:4]=[N:5][C:6]([N:9]2[CH2:14][CH2:13][O:12][CH2:11][CH2:10]2)=[CH:7][CH:8]=1)[NH2:2].[CH3:15][CH2:16][C:17](=O)[CH2:18][CH2:19][C:20](=O)[CH2:21][CH3:22]>C(O)(=O)C>[CH2:21]([C:20]1[N:2]([NH:1][C:3]2[N:4]=[N:5][C:6]([N:9]3[CH2:10][CH2:11][O:12][CH2:13][CH2:14]3)=[CH:7][CH:8]=2)[C:17]([CH2:16][CH3:15])=[CH:18][CH:19]=1)[CH3:22]

参加物

4

反応物 2

HCID 1650543,6-OctanedioneHCID 12603548HCID 12603548、化合物

生成物 1

HCID 23275890HCID 23275890、化合物収率 85.7%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
67 °C

実験手順

To 1.95 g (10 m moles) of 3-hydrazino-6-morpholino-pyridazine dissolved in 12 ml of acetic acid, 1.71 g (12 m moles) of 3,6-octanedione dissolved in 4 ml of acetic acid are added at room temperature. The mixture is heated at 67° C. for 2 hours and then evaporated to dryness under vacuum. The oily residue is dissolved in toluene and the solution is evaporated to dryness. The residue is slurried with ice-water and neutralized with sodium bicarbonate to yield 2.58 g of a solid product. Said material, after crystallization from isopropanol gives 1.25 g (42%) of the title product, melting at 186°-9° C. Elemental analysis, I. R., N.M.R. and mass spectra are in agreement with the assigned structure.

後処理

  1. additionare added at room temperature
  2. customevaporated to dryness under vacuum
  3. dissolutionThe oily residue is dissolved in toluene
  4. customthe solution is evaporated to dryness

出典と根拠

ORDレコード
ord-2577727d135a48c081c88daa4e556844
出典データセット
uspto-grants-1981_01
特許番号
US04247551

反応ノート

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