Reaction equation
C1(=O)[N:5]([CH2:6][C:7]2[CH:16]=[CH:15][C:14]3[C:9](=[CH:10][CH:11]=[C:12]([CH2:17][CH2:18][CH2:19][CH2:20][N:21]([CH2:25][CH2:26][CH3:27])[CH2:22][CH2:23][CH3:24])[CH:13]=3)[CH:8]=2)C(=O)C2=CC=CC=C12>CN.CO>[NH2:5][CH2:6][C:7]1[CH:16]=[CH:15][C:14]2[C:9](=[CH:10][CH:11]=[C:12]([CH2:17][CH2:18][CH2:19][CH2:20][N:21]([CH2:25][CH2:26][CH3:27])[CH2:22][CH2:23][CH3:24])[CH:13]=2)[CH:8]=1Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
The compound (75.0 mg) obtained in Example 124-3 was dissolved in a 40% methylamine/methanol solution (2.0 ml) and stirred overnight at room temperature. After completion of the reaction, the solvent was distilled off and then the residue was added with a 1 mol/l sodium hydroxide aqueous solution and stirred. The solution was subjected to extraction with chloroform and the extract was then washed with saturated saline solution. Subsequently, the organic layer was dried with anhydrous sodium sulfate and the solvent was then distilled off, thereby obtaining the subject compound (67.5 mg) as a colorless oily substance.
Workup
- customAfter completion of the reaction
- distillationthe solvent was distilled off
- additionthe residue was added with a 1 mol/l sodium hydroxide aqueous solution
- stirringstirred
- extractionThe solution was subjected to extraction with chloroform
- washthe extract was then washed with saturated saline solution
- dry with materialSubsequently, the organic layer was dried with anhydrous sodium sulfate
- distillationthe solvent was then distilled off
Sources & evidence
- ORD record
- ord-9c7e9fee8f374433950539a7e56d776f
- Source dataset
- uspto-grants-2010_11
- Patent number
- US07833991B2
Linked notes
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