2-Butanamine, 2-methyl- → HCID 43199060, compound
Reaction equation
Cl.[Cl-].[CH3:3][N:4]([CH3:7])[CH2:5][CH3:6].[C:8]([NH2:13])([CH2:11][CH3:12])([CH3:10])[CH3:9]>>[C:8]([NH:13][CH2:6][CH2:5][N:4]([CH3:7])[CH3:3])([CH2:11][CH3:12])([CH3:10])[CH3:9]Participants
3
Procedure
Into a 300 mL-volume flask equipped with a stirrer and a thermometer were placed 20.6 g (143 mmol) of 2-(dimethylamino)ethane chloride hydrochloride and 74.0 g (859 mmol) of t-pentylamine. And then, the mixture was heated to reflux for 8 hours. After the completion of the reaction, the reaction mixture was filtrated and washed with 100 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (120° C., 11.0 kPa), to provide 13.5 g of 1-t-pentylamino-2-dimethylaminoethane. (Isolation yield: 60%)
Workup
- customInto a 300 mL-volume flask equipped with a stirrer
- temperatureAnd then, the mixture was heated
- temperatureto reflux for 8 hours
- customAfter the completion of the reaction
- filtrationthe reaction mixture was filtrated
- washwashed with 100 ml of hexane twice
- concentrationthe hexane layer was concentrated under reduced pressure
- concentrationThe resultant concentrate
- distillationwas distilled under reduced pressure (120° C., 11.0 kPa)
Sources & evidence
- ORD record
- ord-18f2d0f377bf41a2b7c956520200885d
- Source dataset
- uspto-grants-2014_10
- Patent number
- US08871304B2
Reaction notes
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