Water → 1-(2-Hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene

HRID 1740645

反応式

HRID 1740645 の反応式
Cl[C:2]1[CH:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:21][CH2:22][CH3:23])=[C:15]([O:18][CH2:19][CH3:20])[CH:16]=3)[CH:11]=[C:10]([CH2:24][OH:25])[CH:9]=2)[CH:5]=[CH:4][N:3]=1.C(Cl)Cl.O.O.[NH2:31][NH2:32]>>[NH:31]([C:2]1[CH:7]=[C:6]([C:8]2[C:17]3[C:12](=[CH:13][C:14]([O:21][CH2:22][CH3:23])=[C:15]([O:18][CH2:19][CH3:20])[CH:16]=3)[CH:11]=[C:10]([CH2:24][OH:25])[CH:9]=2)[CH:5]=[CH:4][N:3]=1)[NH2:32]

参加物

5

反応物 4

HCID 962WaterHCID 6344DichloromethaneHCID 24654Hydrazine hydrate (1:1)HCID 220073461-(2-Chloro-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene

生成物 1

HCID 220073321-(2-Hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene

実験手順

A suspension of 1-(2-chloro-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene (3.90 g) in hydrazine hydrate (17.8 ml) is refluxed for 9 hours. The mixture is stirred at room temperature for 10 minutes, and further stirred under ice-cooling for 10 minutes. To the mixture are added methylene chloride and water, and the methylene chloride layer is separated, washed, dried, and concentrated under reduced pressure to remove the solvent. The residue is dissolved in hot ethanol (20 ml), and allowed to cool overnight to give 1-(2-hydrazino-4-pyridyl)-3-hydroxymethyl-6,7-diethoxynaphthalene (3.19 g).

後処理

  1. temperatureis refluxed for 9 hours
  2. stirringfurther stirred under ice-
  3. temperaturecooling for 10 minutes
  4. customthe methylene chloride layer is separated
  5. washwashed
  6. customdried
  7. concentrationconcentrated under reduced pressure
  8. customto remove the solvent
  9. dissolutionThe residue is dissolved in hot ethanol (20 ml)
  10. temperatureto cool overnight

出典と根拠

ORDレコード
ord-a689bc7de4e0433f8340f6eca084bf9f
出典データセット
uspto-grants-1999_10
特許番号
US05969140

関連ノート

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