Methanol → HCID 68870393, compound

HRID 1986595Notes

Reaction equation

HRID 1986595 reaction equation
Cl[C:2]1[C:7]2[N:8]=[CH:9][C:10]3[N:11]([CH2:12][N:13]([O:15][CH3:16])[CH:14]=3)[C:6]=2[N:5]([CH2:17][CH2:18][CH3:19])[CH2:4][C:3]=1[CH3:20].[OH-:21].[K+].O.[CH3:24]O>ClCCl>[CH3:24][O:21][C:2]1[C:7]2[N:8]=[CH:9][C:10]3[N:11]([CH2:12][N:13]([O:15][CH3:16])[CH:14]=3)[C:6]=2[N:5]([CH2:17][CH2:18][CH3:19])[CH2:4][C:3]=1[CH3:20]

Participants

6

Reactant 4

HCID 887MethanolHCID 962WaterHCID 14797Potassium HydroxideHCID 68867784HCID 68867784, compound

Product 1

HCID 68870393HCID 68870393, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

1.5 g of intermediate A1 are dissolved in a mixture of 15 ml methanol and 15 ml dichloromethane. 1 g of solid KOH is added. The mixture is heated up to reflux for 7 hours. At room temperature 30 ml water are added. The organic layer is separated. The aqueous layer is extracted with 20 ml dichloromethane. The unified organic layers are washed with 2×20 ml water. The solvent is removed completely. The residue is purified by LC.

Workup

  1. temperatureThe mixture is heated up
  2. temperatureto reflux for 7 hours
  3. customThe organic layer is separated
  4. extractionThe aqueous layer is extracted with 20 ml dichloromethane
  5. washThe unified organic layers are washed with 2×20 ml water
  6. customThe solvent is removed completely
  7. customThe residue is purified by LC

Sources & evidence

ORD record
ord-379c3ad4c777476f8c63c4372ebe4afa
Source dataset
uspto-grants-2009_06
Patent number
US07550465B2

Reaction notes

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