HCID 802757, compound → HCID 15780690, compound

HRID 1464448Notes

Reaction equation

HRID 1464448 reaction equation
[N+:1]([C:4]1[CH:18]=[C:17]([C:19]([F:22])([F:21])[F:20])[CH:16]=[CH:15][C:5]=1[O:6][C:7]1[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=1[CH:9]=O)([O-])=O.[H][H]>[Ni].C(O)C>[F:20][C:19]([F:22])([F:21])[C:17]1[CH:16]=[CH:15][C:5]2[O:6][C:7]3[CH:14]=[CH:13][CH:12]=[CH:11][C:8]=3[CH2:9][NH:1][C:4]=2[CH:18]=1

Participants

5

Reactant 2

HCID 802757HCID 802757, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 15780690HCID 15780690, compound

Reagents, catalysts & solvents 2

HCID 935NickelCatalystHCID 702EthanolSolvent

Procedure

A solution of 55 parts of the ether obtained in the preceding paragraph in 800 parts of ethanol was hydrogenated over Raney nickel catalyst at room temperature and atmospheric pressure. When hydrogen uptake ceased, the catalyst was removed by filtration and the ethanol solvent was evaporated. The residue was then dissolved in 500 parts by volume of hexane, filtered, and then cooled. There was then obtained yellowish-white crystals which were separated by filtration to give 8-(trifluoromethyl)10,11,-dihydrodibenz -[b,f][1,4]oxazepine melting at about 86°-88° C.

Workup

  1. customthe catalyst was removed by filtration
  2. customthe ethanol solvent was evaporated
  3. dissolutionThe residue was then dissolved in 500 parts by volume of hexane
  4. filtrationfiltered
  5. temperaturecooled
  6. customobtained yellowish-white crystals which were separated by filtration

Sources & evidence

ORD record
ord-f927f12d969d4e5e9bcb6e81d57a4a76
Source dataset
uspto-grants-1994_04
Patent number
US05304644

Reaction notes

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