HCID 802757, compound → HCID 19974016, compound

HRID 1451214Notes

Reaction equation

HRID 1451214 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[CH:9]=[N:1][C:4]=2[CH:18]=1

Participants

5

Reactant 2

HCID 802757HCID 802757, compoundHCID 178418361HCID 178418361, compound

Product 1

HCID 19974016HCID 19974016, 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 is hydrogenated over Raney nickel catalyst at room temperature and atmospheric pressure. When hydrogen uptake ceases the catalyst is removed by filtration and the ethanol solvent is evaporated. The residue is then dissolved in 500 parts by volume of hexane, filtered, and then cooled. There is then obtained yellowish-white crystals which are separated by filtration to give 8-trifluoromethyl-dibenz[b,f][1,4]oxazepine melting at about 86°-88° C.

Workup

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

Sources & evidence

ORD record
ord-384cf096dacd457eb05c0e17e700b735
Source dataset
uspto-grants-1997_02
Patent number
US05604220

Reaction notes

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