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Sodium Hydroxide → 5-Hydroxy-3-phenyl-5-(trifluoromethyl)-4,5-dihydroisoxazole

HRID 332350
Notes
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Reaction equation

HRID 332350 reaction equation
[C:1]([CH2:9][C:10]([C:12]([F:15])([F:14])[F:13])=O)(=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.Cl.[NH2:17][OH:18].[OH-:19].[Na+]>>[C:2]1([C:1]2[CH2:9][C:10]([OH:19])([C:12]([F:13])([F:14])[F:15])[O:18][N:17]=2)[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 3

HCID 14798Sodium HydroxideHCID 675894,4,4-Trifluoro-1-phenyl-1,3-butanedioneHCID 443297Hydroxyamine hydrochloride

Product 1

HCID 28809765-Hydroxy-3-phenyl-5-(trifluoromethyl)-4,5-dihydroisoxazoleYield 91.5%

Procedure

Prepared according to J. Org. Chem., 1995, 60, 3907. A solution of benzoyltrifluoroacetone (21 g, 97 mmol) was added dropwise over 1 h, at 20-30° C., to a solution of hydroxylamine HCl (6.82 g, 98 mmol) containing sodium hydroxide (2 N, 51 mL, 102 mmol) and the resulting mixture heated under reflux for 45 min. After cooling to room temperature, the mixture was poured into ice-water (500 mL), the precipitate was filtered off, washed with water and dried under vacuum to afford the title compound (20.51 g, 91%) which was obtained as a white solid. MS: m/e=230.2 [M−H]−.

Workup

  1. customPrepared
  2. temperaturethe resulting mixture heated
  3. temperatureunder reflux for 45 min
  4. filtrationthe precipitate was filtered off
  5. washwashed with water
  6. customdried under vacuum

Sources & evidence

ORD record
ord-5c703f0561004bd89096f0303a88a4e5
Source dataset
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US08877783B2

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes