Aluminum(III) Chloride → 90060-20-1

HRID 726885Notes

Reaction equation

HRID 726885 reaction equation
[Al+3].[Cl-:2].[Cl-].[Cl-].Cl.C[O:7][C:8]1[C:17]([O:18]C)=[CH:16][CH:15]=[C:14]2[C:9]=1[CH2:10][CH2:11][CH:12]([NH:20][CH3:21])[CH2:13]2>C1(C)C=CC=CC=1>[ClH:2].[OH:7][C:8]1[C:17]([OH:18])=[CH:16][CH:15]=[C:14]2[C:9]=1[CH2:10][CH2:11][CH:12]([NH:20][CH3:21])[CH2:13]2

Participants

4

Reactant 2

HCID 6451240Aluminum(III) ChlorideHCID 19352270HCID 19352270, compound

Product 1

HCID 691848290060-20-1

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent

Procedure

41.4 g of dry AlCl3 (310.4 moles), 230 ml of toluene and 20.0 g of 5,6-dimethoxy-2-methylaminotetralin HCl (77.6 moles) are placed into a 4-necked round-bottomed flask, with stirring, under a slight stream of dry nitrogen. Temperature is brought to 80° C. to obtain a stirrable brown mixture, is left at 80° C. for 4 hours, then cooled to room temperature and poured into ice-water (about 1000 ml total). The aqueous phase is separated and evaporated under vacuum (T about 80° C.). The whitish solid is triturated at room temperature in 750 ml of absolute ethanol, then dried at 60° C. Yield: 16.1 g, 90% (moles), 80% (weight); M.P.>280° C.

Workup

  1. customis brought to 80° C.
  2. customto obtain a stirrable brown mixture
  3. customThe aqueous phase is separated
  4. customevaporated under vacuum (T about 80° C.)
  5. customThe whitish solid is triturated at room temperature in 750 ml of absolute ethanol
  6. customdried at 60° C

Sources & evidence

ORD record
ord-bfd89c90043846da8251a108de6770e6
Source dataset
uspto-grants-1998_01
Patent number
US05710336

Reaction notes

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