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

HRID 1414869노트

반응식

HRID 1414869 반응식
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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
155 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-8be1f7af65f142aa9d65090498c24b6d
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04002753

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