Ethylene Glycol → HCID 22007442、化合物

HRID 324021ノート

反応式

HRID 324021 の反応式
[NH:1]([C:3]1[CH:8]=[C:7]([C:9]2[C:18]3[C:13](=[CH:14][C:15]([O:22][CH3:23])=[C:16]([O:19][CH2:20][CH3:21])[CH:17]=3)[CH:12]=[C:11]([CH2:24][OH:25])[C:10]=2[CH2:26][OH:27])[CH:6]=[CH:5][N:4]=1)[NH2:2].[C:28]([C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][C:32]=1[C:37]([C:39]1[CH:40]=[N:41][CH:42]=[CH:43][CH:44]=1)=O)(O)=[O:29].C(O)CO.C(Cl)[Cl:50]>O>[ClH:50].[N:41]1[CH:42]=[CH:43][CH:44]=[C:39]([C:37]2[C:32]3[C:31](=[CH:36][CH:35]=[CH:34][CH:33]=3)[C:28](=[O:29])[N:1]([C:3]3[CH:8]=[C:7]([C:9]4[C:18]5[C:13](=[CH:14][C:15]([O:22][CH3:23])=[C:16]([O:19][CH2:20][CH3:21])[CH:17]=5)[CH:12]=[C:11]([CH2:24][OH:25])[C:10]=4[CH2:26][OH:27])[CH:6]=[CH:5][N:4]=3)[N:2]=2)[CH:40]=1

参加物

6

反応物 4

HCID 174Ethylene GlycolHCID 6344DichloromethaneHCID 10105136HCID 10105136、化合物HCID 10499321HCID 10499321、化合物

生成物 1

HCID 22007442HCID 22007442、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 1-(2-hydrazino-4-pyridyl)-2,3-bis(hydroxymethyl)-6-methoxy-7-ethoxynaphthalene (2.0 a), (2-carboxyphenyl)-(3-pyridyl) ketone (1.35 g) and ethylene glycol (5 ml) is refluxed for two hours. The mixture under refluxing is cooled to room temperature, and then thereto are added methylene chloride and water. The methylene chloride layer is separated, washed, dried, concentrated under reduced pressure to remove the solvent, and crystallized from chloroform. The precipitated crystals are dissolved in a mixture of chloroform and methanol, and thereto is added a 4 M solution of hydrogen chloride in dioxane (0.67 ml) to give 1-[2-{4-(3-pyridyl)-1(2H)-phthalazinon-2-yl}-4-pyridyl]-2,3-bis(hydroxymethyl)-6-methoxy-7-ethoxynaphthalene hydrochloride (1.43 g), which is listed in Table 10.

後処理

  1. temperatureis refluxed for two hours
  2. temperatureThe mixture under refluxing
  3. customThe methylene chloride layer is separated
  4. washwashed
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customto remove the solvent
  8. customcrystallized from chloroform
  9. dissolutionThe precipitated crystals are dissolved in a mixture of chloroform and methanol
  10. additionis added a 4 M solution of hydrogen chloride in dioxane (0.67 ml)

出典と根拠

ORDレコード
ord-13a462292d214ad48020f5a7c188bfc1
出典データセット
uspto-grants-2001_04
特許番号
US06214996B1

反応ノート

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