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Aluminum(III) Chloride → Chf-1024

HRID 1636640
Notes
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Reaction equation

HRID 1636640 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
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

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

Product 1

HCID 6918482Chf-1024

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.

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-dd9951c61c7245699e83f7923130d322
Source dataset
uspto-grants-2000_03
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06034277

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes