Aluminum(III) Chloride → 167710-00-1

HRID 2293135Notes

Reaction equation

HRID 2293135 reaction equation
Cl.Br[CH2:3][CH2:4][NH:5][CH:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[CH3:14])[CH3:7].[Cl-].[Al+3].[Cl-].[Cl-]>C1C2C(CCCC2)CCC1>[CH3:7][CH:6]1[C:8]2[C:13](=[CH:12][CH:11]=[CH:10][C:9]=2[CH3:14])[CH2:3][CH2:4][NH:5]1

Participants

4

Reactant 2

HCID 6451240Aluminum(III) ChlorideHCID 21476474HCID 21476474, compound

Product 1

HCID 21476500167710-00-1Yield 37.1%

Reagents, catalysts & solvents 1

HCID 7044DecalinSolvent

Conditions

Temperature
0 °C

Procedure

To a mixed solution of 14.7 g of the compound (45.5 mM) prepared in Step 4 above and 100 ml of decaline, was added aluminium chloride and reacted at 140°-150° C. for 1.5 hours, which was cooled to 0° C. The reaction mixture was diluted by pouring into ice water and washed with ethyl ether. The reaction mixture was basified by adding aqueous NaOH solution and the solids produced were filtered. The filtrate was extracted from ethyl ether and the extracts was dried over anhydrous sodium sulfate, concentrated under a reduced pressure, to give 3.16 g of the title compound.

Workup

  1. customreacted at 140°-150° C. for 1.5 hours
  2. additionThe reaction mixture was diluted
  3. washwashed with ethyl ether
  4. additionby adding aqueous NaOH solution
  5. customthe solids produced
  6. filtrationwere filtered
  7. extractionThe filtrate was extracted from ethyl ether
  8. dry with materialthe extracts was dried over anhydrous sodium sulfate
  9. concentrationconcentrated under a reduced pressure

Sources & evidence

ORD record
ord-531df4841b654e1e91d04de2aba01087
Source dataset
uspto-grants-1997_11
Patent number
US05686458

Reaction notes

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