HCID 9909644, compound → HCID 18673899, compound

HRID 1635991Notes

Reaction equation

HRID 1635991 reaction equation
[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[Cl:28])[C:5]([NH:7][C:8]1[CH:9]=[N:10][C:11]([O:14][C:15]2[CH:23]=[CH:22][CH:21]=[C:20]3[C:16]=2[CH2:17][CH2:18][C:19]3=[O:24])=[CH:12][CH:13]=1)=[O:6]>C(OCC)(=O)C.CO.Cl>[ClH:1].[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[Cl:28])[C:5]([NH:7][C:8]1[CH:9]=[N:10][C:11]([O:14][C:15]2[CH:23]=[CH:22][CH:21]=[C:20]3[C:16]=2[CH2:17][CH2:18][C:19]3=[O:24])=[CH:12][CH:13]=1)=[O:6]

Participants

5

Reactant 1

HCID 9909644HCID 9909644, compound

Product 1

HCID 18673899HCID 18673899, compoundYield 183.8%

Reagents, catalysts & solvents 3

HCID 313Hydrochloric AcidSolventHCID 887MethanolSolventHCID 8857Ethyl AcetateSolvent2×

Procedure

After 0.27 g of 3,4-dichloro-N1-(6-[(1-oxo-2,3-dihydro-1H-inden-4-yl)oxy]-3-pyridinyl)benzamide obtained in Example 1 was dissolved in a mixed solvent of 5 ml of ethyl acetate and 2 ml of methanol at a hot state, 1.3 ml of a 4 N solution of hydrogen chloride in ethyl acetate was added to the solution with stirring. Then, the reaction solution was ice-cooled and the deposited crystal was isolated by filtration and dried under reduced pressure to obtain 0.27 g of the titled compound as a white powder. Melting point: 200-207° C.

Workup

  1. additionwas added to the solution
  2. temperaturecooled
  3. customthe deposited crystal was isolated by filtration
  4. customdried under reduced pressure

Sources & evidence

ORD record
ord-c7aaea8af13f4b06986b2d25e9f9ab30
Source dataset
uspto-grants-2003_01
Patent number
US06511995B1

Reaction notes

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