HCID 14556343, compound → HCID 54247497, compound

HRID 1087745Notes

Reaction equation

HRID 1087745 reaction equation
[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH:11](O)[CH2:12][CH2:13][N:14]3[CH2:19][CH2:18][N:17]([C:20]4[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=4)[CH2:16][CH2:15]3)=[CH:10][C:5]=2[O:4][C:3]1=[O:31]>Br>[CH3:1][N:2]1[C:6]2[CH:7]=[CH:8][C:9]([CH:11]=[CH:12][CH2:13][N:14]3[CH2:15][CH2:16][N:17]([C:20]4[CH:25]=[CH:24][CH:23]=[C:22]([C:26]([F:29])([F:28])[F:27])[CH:21]=4)[CH2:18][CH2:19]3)=[CH:10][C:5]=2[O:4][C:3]1=[O:31]

Participants

3

Reactant 1

HCID 14556343HCID 14556343, compound

Product 1

HCID 54247497HCID 54247497, compound

Reagents, catalysts & solvents 1

HCID 260Hydrogen BromideSolvent

Procedure

0.015 mole of 3-methyl-6-{3-[4-(3-trifluoromethylphenyl)-1-piperazinyl]-1-hydroxypropyl}benzoxazolinone is dissolved in 47% strength hydrobromic acid in a 250-cm3 flask, and the solution is stirred at room temperature for 2 hours. The precipitate obtained is drained, washed with acetone, suspended in water and alkalinized with sodium hydroxide. The mixture is extracted several times with chloroform, the organic phases are combined and dried over calcium chloride, filtered and evaporated to dryness on a water bath under vacuum and the base is recrystallized in cyclohexane.

Workup

  1. customThe precipitate obtained
  2. washwashed with acetone
  3. extractionThe mixture is extracted several times with chloroform
  4. dry with materialdried over calcium chloride
  5. filtrationfiltered
  6. customevaporated to dryness on a water bath under vacuum
  7. customthe base is recrystallized in cyclohexane

Sources & evidence

ORD record
ord-2fa7d70531f74bac870e24452812e565
Source dataset
uspto-grants-1990_10
Patent number
US04960778

Reaction notes

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