Acetic Acid → HCID 20378833, compound

HRID 2052172Notes

Reaction equation

HRID 2052172 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 L 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-chloromethylindane are thus obtained in the form of a colourless liquid.

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-5367f9b1dac04b18a38f6dbf13ba3ea9
Source dataset
uspto-grants-1980_01
Patent number
US04182896

Reaction notes

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