Sodium Chloride → Carbazic acid, 3-(6-((2-hydroxyethyl)methylamino)pyridazin-3-YL)-, ethyl ester

HRID 1414869ノート

反応式

HRID 1414869 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([N:8]([CH3:12])[CH2:9][CH2:10][OH:11])=[CH:6][CH:7]=1.[C:13]([NH:18][NH2:19])([O:15][CH2:16][CH3:17])=[O:14].C(=O)([O-])[O-].[K+].[K+].[Cl-].[Na+]>O>[C:13]([NH:18][NH:19][C:2]1[N:3]=[N:4][C:5]([N:8]([CH3:12])[CH2:9][CH2:10][OH:11])=[CH:6][CH:7]=1)([O:15][CH2:16][CH3:17])=[O:14]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 11430Potassium CarbonateHCID 20064Hydrazinecarboxylic acid, ethyl esterHCID 122375892-[(6-Chloropyridazin-3-yl)(methyl)amino]ethan-1-ol

生成物 1

HCID 41014Carbazic acid, 3-(6-((2-hydroxyethyl)methylamino)pyridazin-3-YL)-, ethyl ester

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
155 °C

実験手順

A mixture of 1.87 g (0.01 moles) 3-chloro-6-[N-(2-hydroxyethyl)-methylamino]-pyridazine and 2.08 g (0.02 moles) monocarbethoxyhydrazine is warmed up to 155° C and kept at this temperature for half an hour. The product is cooled and dissolved in water, alkalinized by addition of solid potassium carbonate and the aqueous solution saturated by adding sodium chloride. A flocky precipitate separates which is subsequently collected by filtration and crystallized from ethanol, to give with good yields 3-(2-carbethoxyhydrazino)-6-[N-(2-hydroxyethyl)methylamino] -pyridazine melting at 131°-133° C. I.R. Spectrum (mineral oil, cm-1); 3320-3080 (OH and NH), 1715 (C=O carbamate), 1500 (pyridazinic ring), 840 (two ortho aromatic hydrogens).

後処理

  1. waitkept at this temperature for half an hour
  2. temperatureThe product is cooled
  3. filtrationA flocky precipitate separates which is subsequently collected by filtration
  4. customcrystallized from ethanol
  5. customto give

出典と根拠

ORDレコード
ord-8be1f7af65f142aa9d65090498c24b6d
出典データセット
uspto-grants-1977_01
特許番号
US04002753

反応ノート

読み込み中…