Ethanol → HCID 19081375, compound

HRID 963189Notes

Reaction equation

HRID 963189 reaction equation
C(O)C.[C:4]([N:8]1[C:13](=[O:14])[C:12]([C:15]([O:17][CH3:18])=[O:16])=[C:11](Cl)[CH:10]=[N:9]1)([CH3:7])([CH3:6])[CH3:5].[N:20]1[CH:25]=[CH:24][C:23]([CH2:26][NH2:27])=[CH:22][CH:21]=1>C(N(CC)CC)C>[C:4]([N:8]1[C:13](=[O:14])[C:12]([C:15]([O:17][CH3:18])=[O:16])=[C:11]([NH:27][CH2:26][C:23]2[CH:24]=[CH:25][N:20]=[CH:21][CH:22]=2)[CH:10]=[N:9]1)([CH3:7])([CH3:6])[CH3:5]

Participants

5

Reactant 3

HCID 702EthanolHCID 773174-PyridinemethanamineHCID 19081400HCID 19081400, compound

Product 1

HCID 19081375HCID 19081375, compound

Reagents, catalysts & solvents 1

HCID 8471TriethylamineSolvent

Procedure

7 ml of an absolute ethanol solution of 170 mg of 2-tert-butyl-5-chloro-4-methoxycarbonylpyridazin-3-(2H)-one, 76 mg of 4-picolylamine and 80 mg of triethylamine, was reacted for 4 hours under heating and refluxing and then left to cool. Ethanol was distilled off under reduced pressure, and 0.3 g of the obtained oil was subjected to column chromatography. Using an eluent (ethyl acetate:methanol=20:1), 0.13 g of the desired product (Compound No. 22) having a melting point of from 99° to 100° C., was obtained.

Workup

  1. temperatureunder heating
  2. temperaturerefluxing
  3. waitleft
  4. temperatureto cool
  5. distillationEthanol was distilled off under reduced pressure, and 0.3 g of the obtained oil
  6. customof from 99° to 100° C.
  7. customwas obtained

Sources & evidence

ORD record
ord-8a4728635f294d9cad2c7e36cc38ed0b
Source dataset
uspto-grants-1998_06
Patent number
US05763439

Reaction notes

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