Ethanol → HCID 85813005, compound

HRID 1284281Notes

Reaction equation

HRID 1284281 reaction equation
[F:1][C:2]([C:13]1[CH:18]=[CH:17][C:16]([C:19](=O)[CH3:20])=[CH:15][CH:14]=1)([F:12])[C:3]([F:11])([F:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.Cl.[NH2:23][OH:24].C(O)C>N1C=CC=CC=1>[F:1][C:2]([C:13]1[CH:18]=[CH:17][C:16]([C:19](=[N:23][OH:24])[CH3:20])=[CH:15][CH:14]=1)([F:12])[C:3]([F:11])([F:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1

Participants

5

Reactant 3

HCID 702EthanolHCID 443297Hydroxyamine hydrochlorideHCID 203722211-[4-(1,1,2,2-Tetrafluoro-2-phenylethyl)phenyl]ethan-1-one

Product 1

HCID 85813005HCID 85813005, compound

Reagents, catalysts & solvents 1

HCID 1049PyridineSolvent

Procedure

A solution of 1.1 g. (0.00372 mole) of 4'-(α,α,β,β-tetrafluorophenethyl)-acetophenone, 0.7 g. (0.0071 mole) of hydroxylamine hydrochloride, 8.5 ml. of absolute ethanol, and 1.5 ml. of dry pyridine is heated to refluxing for 6 hours. Solvents are evaporated under reduced pressure and the residual solid is triturated with water. The crystalline product, m.p. 137°-139°C., is collected and recrystallized from hexane to obtain white needles, m.p. 139°-141°C. Recrystallization from hexane affords the analytical sample, m.p. 140°-141°C.

Workup

  1. temperatureto refluxing for 6 hours
  2. customSolvents are evaporated under reduced pressure
  3. customthe residual solid is triturated with water
  4. customThe crystalline product, m.p. 137°-139°C., is collected
  5. customrecrystallized from hexane
  6. customto obtain white needles, m.p. 139°-141°C
  7. customRecrystallization from hexane
  8. customaffords the analytical sample, m.p. 140°-141°C.

Sources & evidence

ORD record
ord-0df20a91b6524262a0800dc41cf86db8
Source dataset
uspto-grants-1976_08
Patent number
US03978127

Reaction notes

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