Hydrochloric Acid → HCID 69053915, compound

HRID 1867564Notes

Reaction equation

HRID 1867564 reaction equation
Cl.[Br:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[N:13]([C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=3[Cl:21])[N:12]=[C:11]([C:22]([NH:24][NH:25]C(OC(C)(C)C)=O)=[O:23])[C:10]=2[CH2:33][CH3:34])=[CH:5][CH:4]=1>CO>[Br:2][C:3]1[CH:4]=[CH:5][C:6]([C:9]2[N:13]([C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=3[Cl:21])[N:12]=[C:11]([C:22]([NH:24][NH2:25])=[O:23])[C:10]=2[CH2:33][CH3:34])=[CH:7][CH:8]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 86618351HCID 86618351, compound

Product 1

HCID 69053915HCID 69053915, compoundYield 79.8%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Conditions

Temperature
40 °C

Procedure

40 ml of 2N ethereal hydrochloric acid are added to a solution of 12.7 g of the compound obtained in stage B in 200 ml of MeOH and the mixture is then heated at 40° C. for 3 hours. The reaction mixture is concentrated under vacuum, the residue is extracted with ether, the organic phase is washed twice with a 10% NaHCO3 solution and dried over MgSO4, and the solvent is evaporated under vacuum. 8.3 g of the expected compound are obtained after crystallization from an ether/pentane mixture.

Workup

  1. concentrationThe reaction mixture is concentrated under vacuum
  2. extractionthe residue is extracted with ether
  3. washthe organic phase is washed twice with a 10% NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. customthe solvent is evaporated under vacuum

Sources & evidence

ORD record
ord-e63f86a3789e4db18ff369d404b073e5
Source dataset
uspto-grants-2009_12
Patent number
US07632852B2

Reaction notes

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