60423-91-8 → HCID 22457011, compound

HRID 1076340Notes

Reaction equation

HRID 1076340 reaction equation
[CH3:1][CH:2]([CH2:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]#[N:14])=[CH:9][CH:8]=1)[C:3]([OH:5])=O>O>[C:13]([C:10]1[CH:11]=[C:12]2[C:7]([CH2:6][CH:2]([CH3:1])[C:3]2=[O:5])=[CH:8][CH:9]=1)#[N:14]

Participants

3

Reactant 1

HCID 2153991960423-91-8

Product 1

HCID 22457011HCID 22457011, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

α-Methyl-β-(p-cyanophenyl)propionic acid (14.5 g.) is added to 170 g. of polyphosphoric acid at 50° and the mixture is heated at 83°-90° for two hours. The syrup is poured into iced water, stirred for one-half hour and then extracted with ether three times. The ether solution is washed with water twice and 5% NaHCO3 five times until all the acidic material has been removed. The remaining neutral solution is washed with water and dried over sodium sulfate. Evaporation of the solution gives the indanone, m.p. 95°-95°.

Workup

  1. extractionextracted with ether three times
  2. washThe ether solution is washed with water twice
  3. custom5% NaHCO3 five times until all the acidic material has been removed
  4. washThe remaining neutral solution is washed with water
  5. dry with materialdried over sodium sulfate
  6. customEvaporation of the solution

Sources & evidence

ORD record
ord-8a7ac25bc587446d817acec1909c2f3f
Source dataset
uspto-grants-1976_05
Patent number
US03956363

Reaction notes

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