Phosphoric Acid → HCID 22418013, compound
Reaction equation
[NH2:1][C:2]1[C:7]([NH2:8])=[C:6]([CH2:9][CH2:10][CH3:11])[CH:5]=[CH:4][N:3]=1.[C:12](O)(=O)[CH2:13][CH3:14].P(=O)(O)(O)O.[OH-].[Na+]>>[CH2:13]([C:14]1[NH:8][C:7]2[C:2]([N:1]=1)=[N:3][CH:4]=[CH:5][C:6]=2[CH2:9][CH2:10][CH3:11])[CH3:12]Participants
5
Procedure
2.6 g (0.017M) of 2,3-diamino-4-n-propylpyridine and 1.4 ml (0.019M) of propionic acid were added to 15 ml of phosphoric acid, and the mixture was heated at 140° to 150° C. for 20 hr. It was cooled to room temperature, poured into a cold aqueous NaOH solution and then extracted with ethyl acetate. The extract was dried over magnesium sulfate, and the solvent was distilled off in vacuo to prepare a substantially pure brown oleaginous intended product. The yield was 2.9 g (this compound was used as a starting material in the preparation of the following raw material (29)).
Workup
- temperaturethe mixture was heated at 140° to 150° C. for 20 hr
- extractionextracted with ethyl acetate
- dry with materialThe extract was dried over magnesium sulfate
- distillationthe solvent was distilled off in vacuo
- customto prepare a substantially pure brown oleaginous intended product
Sources & evidence
- ORD record
- ord-53eff9cecaa249a0b6d3aa100718ee80
- Source dataset
- uspto-grants-1994_03
- Patent number
- US05298518
Reaction notes
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