Ethanol → HCID 18951062, compound

HRID 2248268Notes

Reaction equation

HRID 2248268 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH:12]2[CH2:24][C:23]3[C:22]4[C:17](=[CH:18][C:19]([F:26])=[CH:20][C:21]=4[F:25])[N:16]([CH2:27]CC#N)[C:15]=3[CH2:14][CH2:13]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[OH-:31].[Na+].[CH2:33]([OH:35])[CH3:34]>>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][CH:12]2[CH2:24][C:23]3[C:22]4[C:17](=[CH:18][C:19]([F:26])=[CH:20][C:21]=4[F:25])[N:16]([CH2:27][CH2:34][C:33]([OH:31])=[O:35])[C:15]=3[CH2:14][CH2:13]2)(=[O:10])=[O:9])=[CH:4][CH:3]=1

Participants

4

Reactant 3

HCID 702EthanolHCID 14798Sodium HydroxideHCID 18951061HCID 18951061, compound

Product 1

HCID 18951062HCID 18951062, compound

Procedure

3.05 g (6.8 mmol) of the compound from Example III are dissolved in 20 ml of ethanol, 100 ml of 10% strength sodium hydroxide solution are added, and the mixture is then stirred under reflux for 16 hours. The cooled batch is extracted by shaking twice using 50 ml of methylene chloride each time, and a pH of 1 is established at 0° C., using 6 N hydrochloric acid. The precipitate which has separated out is filtered off with suction, washed with water to neutrality, dried in a high vacuum over phosphorus pentoxide and sodium hydroxide, and weighed.

Workup

  1. temperatureunder reflux for 16 hours
  2. extractionThe cooled batch is extracted
  3. stirringby shaking twice
  4. customis established at 0° C.
  5. customThe precipitate which has separated out
  6. filtrationis filtered off with suction
  7. washwashed with water to neutrality
  8. dry with materialdried in a high vacuum over phosphorus pentoxide and sodium hydroxide

Sources & evidence

ORD record
ord-d6d7292e53aa4e478a6a44de7756378e
Source dataset
uspto-grants-1991_08
Patent number
US05039670

Reaction notes

Loading…