Ethylene Glycol → HCID 22007442, 화합물

HRID 613018노트

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HRID 613018 반응식
[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

참가 물질

6

반응물 4

HCID 174Ethylene GlycolHCID 6344DichloromethaneHCID 10105136HCID 10105136, 화합물HCID 10499321HCID 10499321, 화합물

생성물 1

HCID 22007442HCID 22007442, 화합물

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1-(2-hydrazino-4-pyridyl)-2,3-bis(hydroxymethyl)-6-methoxy-7-ethoxynaphthalene (2.0 g), (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.

후처리

  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)

출처 및 근거

ORD 기록
ord-868563f7e6f644ac951c060ee93edb3b
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06005106

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