Hydrochloric Acid → HCID 18175107, compound

HRID 395584Notes

Reaction equation

HRID 395584 reaction equation
[C:1]1([CH2:7][C:8]([NH:10][CH2:11][CH2:12][CH:13]2[C:22]3[C:17](=[CH:18][CH:19]=[C:20]([C:23]([NH:25][CH2:26][C:27](Cl)=[O:28])=[O:24])[CH:21]=3)[O:16][CH2:15][CH2:14]2)=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[Cl-].[Al+3].[Cl-].[Cl-].Cl>ClC(Cl)C(Cl)Cl>[O:28]=[C:27]1[C:21]2[C:22]3[CH:13]([CH2:12][CH2:11][NH:10][C:8](=[O:9])[CH2:7][C:1]4[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=4)[CH2:14][CH2:15][O:16][C:17]=3[CH:18]=[CH:19][C:20]=2[C:23](=[O:24])[NH:25][CH2:26]1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 6451240Aluminum(III) ChlorideHCID 18175096HCID 18175096, compound

Product 1

HCID 18175107HCID 18175107, compound

Reagents, catalysts & solvents 1

HCID 65911,1,2,2-TetrachloroethaneSolvent

Conditions

Temperature
60 °C

Procedure

The product obtained in Step B (3 mmol), dissolved in 1,1,2,2-tetrachloroethane (30 ml), is added dropwise to a solution of aluminium chloride (10 mmol) in the same solvent (20 ml) under nitrogen. The reaction mixture is heated at 60° C., with stirring, until the reaction has ceased. The solution is then poured into a mixture of ice (10 g)/concentrated HCl (0.3 ml) and stirring is carried out for one hour. The aqueous phase is extracted twice with chloroform; the combined organic phases are then dried over magnesium sulphate and concentrated under reduced pressure. The residue is chromatographed on silica gel to yield the title product.

Workup

  1. stirringstirring
  2. extractionThe aqueous phase is extracted twice with chloroform
  3. dry with materialthe combined organic phases are then dried over magnesium sulphate
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is chromatographed on silica gel

Sources & evidence

ORD record
ord-613fcd5c4e0141bb8b38ea58b7f0bcd7
Source dataset
uspto-grants-2003_08
Patent number
US06605632B1

Reaction notes

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