Water → HCID 14461327, compound

HRID 1086820Notes

Reaction equation

HRID 1086820 reaction equation
[CH2:1]([O:3][C:4]([CH:6]([C:30](=O)[CH:31]([CH3:33])[CH3:32])[CH:7]([C:16]1[CH:21]=[CH:20][C:19]([F:22])=[C:18]([O:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:17]=1)[C:8]([C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)=[O:9])=[O:5])[CH3:2].O.O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[CH2:1]([O:3][C:4]([C:6]1[C:7]([C:16]2[CH:21]=[CH:20][C:19]([F:22])=[C:18]([O:23][C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH:17]=2)=[C:8]([C:10]2[CH:11]=[CH:12][CH:13]=[CH:14][CH:15]=2)[O:9][C:30]=1[CH:31]([CH3:32])[CH3:33])=[O:5])[CH3:2]

Participants

5

Reactant 3

HCID 962Water2×HCID 521998p-Toluenesulfonic acid monohydrateHCID 14461326HCID 14461326, compound

Product 1

HCID 14461327HCID 14461327, compound

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

185 g (0.4 mmol) of the compound from Example 22 are boiled in a water separator for 2.5 hours with 15.2 g (0.05 mol) of p-toluenesulphonic acid hydrate in 2 l of toluene. 7 ml of water separates from the mixture. After cooling, the mixture is washed twice with saturated bicarbonate solution and once with sodium chloride solution, dried over sodium sulphate and concentrated to dryness. The residue is recrystallized from ethanol.

Workup

  1. temperatureAfter cooling
  2. washthe mixture is washed twice with saturated bicarbonate solution and once with sodium chloride solution
  3. dry with materialdried over sodium sulphate
  4. concentrationconcentrated to dryness
  5. customThe residue is recrystallized from ethanol

Sources & evidence

ORD record
ord-40085627b6ac4a6f91e094d868911077
Source dataset
uspto-grants-1991_07
Patent number
US05032590

Reaction notes

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