p-Toluenesulfonic acid monohydrate → HCID 15130942, compound

HRID 1613616Notes

Reaction equation

HRID 1613616 reaction equation
[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:12][CH2:11][CH2:10][CH2:9][CH:8](O)[C:7]=2[CH:14]=1)#[N:2].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C1(C)C=CC=CC=1>[C:1]([C:3]1[CH:4]=[CH:5][C:6]2[O:12][CH2:11][CH2:10][CH:9]=[CH:8][C:7]=2[CH:14]=1)#[N:2]

Participants

4

Reactant 2

HCID 521998p-Toluenesulfonic acid monohydrateHCID 15130941HCID 15130941, compound

Product 1

HCID 15130942HCID 15130942, compoundYield 95.2%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

18.9 g (0.1 mole) of 7-cyano-5-hydroxy-2,3,4,5-tetrahydro-1-benzoxepin are heated with 0.3 g of p-toluenesulfonic acid monohydrate in toluene with a water trap for 1.5 hours. After the solution has cooled it is washed with 1N potassium bicarbonate solution, water and saturated sodium chloride solution and, after drying over sodium sulfate, the solvent is evaporated off in vacuo. 16.3 g of solid of melting point 69°-71° C. are obtained.

Workup

  1. temperatureAfter the solution has cooled it
  2. washis washed with 1N potassium bicarbonate solution, water and saturated sodium chloride solution
  3. dry with materialafter drying over sodium sulfate
  4. customthe solvent is evaporated off in vacuo

Sources & evidence

ORD record
ord-4548dfd1a776416181b7e9ebcd46b192
Source dataset
uspto-grants-1993_03
Patent number
US05194442

Reaction notes

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