Hydrochloric Acid → HCID 58011742, compound

HRID 660849Notes

Reaction equation

HRID 660849 reaction equation
[CH:1]1([NH:4][C:5]([NH:7][NH:8][C:9](=O)[C:10]2[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=2[F:17])=[O:6])[CH2:3][CH2:2]1.Cl>[OH-].[Na+].O>[CH:1]1([N:4]2[C:9]([C:10]3[CH:15]=[CH:14][C:13]([F:16])=[CH:12][C:11]=3[F:17])=[N:8][NH:7][C:5]2=[O:6])[CH2:3][CH2:2]1

Participants

5

Procedure

1.00 g (3.92 mmol) of N-cyclopropyl-2-(2,4-difluorobenzoyl)-hydrazinecarboxamide from Example 5A are heated under reflux in 4 ml 4 N aqueous sodium hydroxide for 28 hrs. After cooling, it is acidified to about pH 2 with 2 N hydrochloric acid, diluted with water and extracted four times with ethyl acetate. The combined organic phases are dried over magnesium sulphate, filtered, concentrated and the residue dried in vacuo. 0.415 g (31% of theory) of the target compound are thus obtained, which is further reacted as such.

Workup

  1. temperatureAfter cooling
  2. extractionextracted four times with ethyl acetate
  3. dry with materialThe combined organic phases are dried over magnesium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customthe residue dried in vacuo
  7. custom0.415 g (31% of theory) of the target compound are thus obtained
  8. customwhich is further reacted as such

Sources & evidence

ORD record
ord-ec8084ce9ed64f8281fcd92877460381
Source dataset
uspto-grants-2011_12
Patent number
US08084481B2

Reaction notes

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