Methylamine ethanol → HCID 66642638, compound
Reaction equation
[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4](N(C)C=O)[CH:3]=1.[CH2:18]([OH:20])C.[CH3:21][NH2:22]>>[Cl:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([O:12][CH3:13])[CH:10]=2)[N:5]=[C:4]([C:18]([NH:22][CH3:21])=[O:20])[CH:3]=1Participants
3
Procedure
Embodiment 6: Preparation of 4-chloro-6-methoxyl-N-methyl-2-quinolinyl formamide 10 g of 4-chloro-6-methoxyquinolinyl-2-carbonyl chloride (obtained from embodiment 1) was reacted with 200 ml of 2M methylamine ethanol solution under 0° C. for 36 hours until the reaction finished. The solvent was evaporated under vacuum and the residues were added with water followed by stirring evenly. Ethyl acetate was added for extracting and the ethyl acetate layer was dried with anhydrous sodium sulfate. The ethyl acetate layer was removed under vacuum to obtain 9 g of 4-chloro-6-methoxy-N-methyl-2-quinoline carboxamide.
Workup
- customThe solvent was evaporated under vacuum
- additionthe residues were added with water
- additionEthyl acetate was added
- extractionfor extracting
- dry with materialthe ethyl acetate layer was dried with anhydrous sodium sulfate
- customThe ethyl acetate layer was removed under vacuum
Sources & evidence
- ORD record
- ord-3ef4a321b7aa449eb46bf972af1fa6a3
- Source dataset
- uspto-grants-2015_02
- Patent number
- US08957087B2
Reaction notes
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