Hydrochloric Acid → HCID 67549403, compound

HRID 1890799Notes

Reaction equation

HRID 1890799 reaction equation
[Cl:1][C:2]1[CH:13]=[CH:12][C:5]([O:6][C:7]([CH3:11])([CH3:10])[C:8]#[N:9])=[C:4]([F:14])[CH:3]=1.Cl.[CH2:16]([OH:18])[CH3:17]>ClCCl>[ClH:1].[Cl:1][C:2]1[CH:13]=[CH:12][C:5]([O:6][C:7]([CH3:11])([CH3:10])[C:8](=[NH:9])[O:18][CH2:16][CH3:17])=[C:4]([F:14])[CH:3]=1

Participants

5

Reactant 3

HCID 313Hydrochloric AcidHCID 702EthanolHCID 57467473HCID 57467473, compound

Product 1

HCID 67549403HCID 67549403, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

Through a cooled solution of Example 53D (7.2 g, 33.7 mmol) in ethanol (75 mL) and dichloromethane (30 mL) was bubbled HCl gas at 0° C. for 30 minutes. The reaction was kept in a refrigerator for 24-72 hours (checked by LCMS). The reaction mixture was then concentrated and the residue was triturated with diethyl ether. The titled compound was collected by filtration.

Workup

  1. concentrationThe reaction mixture was then concentrated
  2. customthe residue was triturated with diethyl ether
  3. filtrationThe titled compound was collected by filtration

Sources & evidence

ORD record
ord-ae7a1300402e4c4ca36437844c00146c
Source dataset
uspto-grants-2013_08
Patent number
US08507493B2

Reaction notes

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