Acetic Acid → HCID 20378833, compound

HRID 1834213Notes

Reaction equation

HRID 1834213 reaction equation
[CH3:1][CH:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]([CH3:11])[CH2:3]1.[C:12](O)(=O)C.P(=O)(O)(O)O.[ClH:21]>O>[CH3:11][CH:4]1[C:5]2[C:10](=[CH:9][C:8]([CH2:12][Cl:21])=[CH:7][CH:6]=2)[CH:2]([CH3:1])[CH2:3]1

Participants

6

Reactant 4

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 1004Phosphoric AcidHCID 201431,3-Dimethyl-2,3-dihydro-1H-indene

Product 1

HCID 20378833HCID 20378833, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

a mixture of 73 g of 1,3-dimethyl-indane, 28 g of trioxymethylene, 64 ml of acetic acid, 41 ml of 85% strength phosphoric acid and 100 ml of concentrated hydrochloric acid is stirred for 24 hours at between 58° and 60° C. The reaction mixture is taken up in a mixture of water and ice and the organic products are extracted with ether. The ether phase is washed with water and dried over sodium sulphate. After evaporation of the ether, the residue obtained is distilled in vacuo. 44.8 g of 1,3-dimethyl-5-chloromethyl-indane are thus obtained in the form of a colourless liquid. Boiling point 1 mm Hg = 110° C.

Workup

  1. extractionthe organic products are extracted with ether
  2. washThe ether phase is washed with water
  3. dry with materialdried over sodium sulphate
  4. customAfter evaporation of the ether
  5. customthe residue obtained
  6. distillationis distilled in vacuo

Sources & evidence

ORD record
ord-b18046a240fe473fb1554176d1c578c9
Source dataset
uspto-grants-1978_01
Patent number
US04069326

Reaction notes

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