Hydrochloric Acid → HCID 58042801, compound

HRID 564086Notes

Reaction equation

HRID 564086 reaction equation
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][CH2:6][C:7](=[O:10])[CH2:8]Cl.[CH2:11]1[C:19]2[C:14](=[CH:15]C=[CH:17][CH:18]=2)[CH2:13][N:12]1[C:20](=[O:25])[C:21]([F:24])([F:23])[F:22].Cl>ClCCCl>[Cl:5][CH2:6][C:7]([C:8]1[CH:15]=[C:14]2[C:19](=[CH:18][CH:17]=1)[CH2:11][N:12]([C:20](=[O:25])[C:21]([F:23])([F:24])[F:22])[CH2:13]2)=[O:10]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 107931,3-DichloroacetoneHCID 6451240Aluminum(III) ChlorideHCID 21766494HCID 21766494, compound

Product 1

HCID 58042801HCID 58042801, compound

Reagents, catalysts & solvents 1

HCID 111,2-DichloroethaneSolvent2×

Procedure

To 5.00 g (37.5 mmol) aluminium(III)-chloride in 20 mL 1,2-dichloroethane is added at 0° C. dropwise 2.24 mL (28.1 mmol) 1,3-dichloro-propan-2-one keeping the temperature below 15° C. Then 4.48 g (18.7 mmol) 1-(1,3-dihydro-isoindol-2-yl)-2,2,2-trifluoro-ethanone in 5 mL 1,2-dichloroethane is added dropwise at RT keeping the temperature between 40-45° C. The reaction is stirred for 18 h at RT and is poured onto aqueous HCl-solution. The aqueous phase is extracted twice with DCM, the organic phase is washed with water, dried over MgSO4, filtered and the solvent is evaporated. The residue is elutriated with PE and the precipitate is collected.

Workup

  1. custombetween 40-45° C
  2. extractionThe aqueous phase is extracted twice with DCM
  3. washthe organic phase is washed with water
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customthe solvent is evaporated
  7. customthe precipitate is collected

Sources & evidence

ORD record
ord-c7a062b9fb2246018f4a28707b8cd444
Source dataset
uspto-grants-2011_11
Patent number
US08067590B2

Reaction notes

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